#------------------------------------------------------------------------------
#$Date: 2024-09-06 02:14:05 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294425 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/35/7133514.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7133514
loop_
_publ_author_name
'Pennachio, Matthew'
'Wei, Zheng'
'Mamada, Masashi'
'Frigoli, Michel'
'Petrukhina, Marina A.'
_publ_section_title
;
 Chemical reduction of π-expanded functionalized pentacene:
 cooperation of side group in alkali metal binding.
;
_journal_issue                   71
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9526
_journal_page_last               9529
_journal_paper_doi               10.1039/d4cc03318c
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C80 H104 Na2 O6 Si2'
_chemical_formula_sum            'C80 H104 Na2 O6 Si2'
_chemical_formula_weight         1263.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2022-04-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-07-02 deposited with the CCDC.	2024-08-08 downloaded from the CCDC.
;
_cell_angle_alpha                97.3160(10)
_cell_angle_beta                 100.1920(10)
_cell_angle_gamma                100.4480(10)
_cell_formula_units_Z            1
_cell_length_a                   7.7756(2)
_cell_length_b                   14.1848(4)
_cell_length_c                   16.3912(5)
_cell_measurement_reflns_used    9783
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.13
_cell_measurement_theta_min      2.45
_cell_volume                     1725.94(9)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'APEX3 v.2018.7-2 (Bruker AXS Inc., 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Pilatus1M(CdTe) pixel array detector'
_diffrn_detector_area_resol_mean 30
_diffrn_detector_type            'CMOS pixel array detector'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  'APS_15-ID-D xHuber Kappa'
_diffrn_measurement_method       'phi rotation'
_diffrn_radiation_collimation    '0.2 mm sinlge-pinhole'
_diffrn_radiation_monochromator  'Si(111) & Si(311)'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.41328
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0321
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.930
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            115112
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.930
_diffrn_reflns_theta_full        14.357
_diffrn_reflns_theta_max         22.173
_diffrn_reflns_theta_min         1.041
_diffrn_source                   synchrotron
_diffrn_source_current           103.0
_diffrn_source_power             103.0
_diffrn_source_type
'Insertion Device, Station 15 ID-B, APS, Argonne Nat'l Lab'
_diffrn_source_voltage           1000.0
_exptl_absorpt_coefficient_mu    0.042
_exptl_absorpt_correction_T_max  0.7447
_exptl_absorpt_correction_T_min  0.5886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction.
wR2(int) was 0.0854 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.7904.
The λ/2 correction factor is not present.
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             682
_exptl_crystal_size_max          0.013
_exptl_crystal_size_mid          0.009
_exptl_crystal_size_min          0.008
_refine_diff_density_max         0.657
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         20479
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0567
_refine_ls_R_factor_gt           0.0433
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0747P)²+0.1346P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1318
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15721
_reflns_number_total             20479
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03318c2.cif
_cod_data_source_block           Na2_TIPS_PPP
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas 

 Adding full bibliography for 7133514.cif.
;
_cod_original_cell_volume        1725.94(8)
_cod_database_code               7133514
_shelx_shelxl_version_number     2019/2
_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.
;
_shelx_estimated_absorpt_t_max   1.000
_shelx_estimated_absorpt_t_min   0.999
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Si1-C23 \\sim Si1-C23X
 with sigma of 0.02
 C23-C24 \\sim C23X-C25X
 with sigma of 0.02
 C23-C25 \\sim C23X-C24X
 with sigma of 0.02
 C24-C25 \\sim C25X-C24X
 with sigma of 0.04
 Si1-C24 \\sim Si1-C25X
 with sigma of 0.04
 Si1-C25 \\sim Si1-C24X
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C23 \\sim C24 \\sim C25 \\sim C23X \\sim C24X \\sim C25X: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02 within 2A
Uanis(C23X) = Uanis(C23)
4. Rigid body (RIGU) restrains
 Si1, C23, C24, C25, C23X, C24X, C25X
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C23X)=Sof(H23X)=Sof(C24X)=Sof(H24D)=Sof(H24E)=Sof(H24F)=Sof(C25X)=
 Sof(H25D)=Sof(H25E)=Sof(H25F)=1-FVAR(1)
 Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=FVAR(1)
6.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C23X(H23X)
6.b Secondary CH2 refined with riding coordinates:
 C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C33(H33A,
 H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B), C37(H37A,H37B),
 C38(H38A,H38B), C39(H39A,H39B), C40(H40A,H40B)
6.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C12(H12)
6.d Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C24X(H24D,H24E,H24F),
 C25X(H25D,H25E,H25F)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Si1 Si 0.25848(3) 0.05406(2) 0.23896(2) 0.01865(4) Uani 1 1 d D . . . .
Na1 Na 0.15807(4) 0.38475(2) 0.27303(2) 0.02378(6) Uani 1 1 d . . . . .
O1 O 0.14156(9) 0.54204(4) 0.28077(4) 0.03070(11) Uani 1 1 d . . . . .
O2 O 0.03214(8) 0.33833(4) 0.13557(3) 0.02566(9) Uani 1 1 d . . . . .
O3 O -0.06985(9) 0.33641(5) 0.33443(4) 0.03342(12) Uani 1 1 d . . . . .
C1 C 0.52897(8) 0.54116(3) 0.48085(3) 0.01457(8) Uani 1 1 d . . . . .
C2 C 0.57360(8) 0.63580(4) 0.53000(3) 0.01531(8) Uani 1 1 d . . . . .
C3 C 0.62749(8) 0.71538(4) 0.49161(4) 0.01743(9) Uani 1 1 d . . . . .
H3 H 0.656681 0.778730 0.523979 0.021 Uiso 1 1 calc R U . . .
C4 C 0.63975(8) 0.70480(4) 0.40757(3) 0.01687(9) Uani 1 1 d . . . . .
C5 C 0.69115(10) 0.78697(4) 0.36868(4) 0.02071(10) Uani 1 1 d . . . . .
H5 H 0.723045 0.850031 0.401626 0.025 Uiso 1 1 calc R U . . .
C6 C 0.69548(10) 0.77710(4) 0.28592(4) 0.02187(11) Uani 1 1 d . . . . .
H6 H 0.728188 0.833443 0.261776 0.026 Uiso 1 1 calc R U . . .
C7 C 0.65183(9) 0.68359(4) 0.23407(4) 0.01861(9) Uani 1 1 d . . . . .
C8 C 0.65464(10) 0.67240(4) 0.14821(4) 0.02149(10) Uani 1 1 d . . . . .
H8 H 0.685998 0.727828 0.122720 0.026 Uiso 1 1 calc R U . . .
C9 C 0.61164(9) 0.58044(4) 0.10067(4) 0.02078(10) Uani 1 1 d . . . . .
H9 H 0.613660 0.573159 0.042448 0.025 Uiso 1 1 calc R U . . .
C10 C 0.56562(9) 0.49872(4) 0.13676(4) 0.01862(9) Uani 1 1 d . . . . .
H10 H 0.537204 0.436273 0.102858 0.022 Uiso 1 1 calc R U . . .
C11 C 0.56021(8) 0.50645(4) 0.22233(3) 0.01644(8) Uani 1 1 d . . . . .
C12 C 0.51137(8) 0.42494(4) 0.26099(3) 0.01705(9) Uani 1 1 d . . . . .
H12 H 0.485713 0.361884 0.228276 0.020 Uiso 1 1 calc R U . . .
C13 C 0.49946(8) 0.43360(4) 0.34521(3) 0.01528(8) Uani 1 1 d . . . . .
C14 C 0.54319(8) 0.52901(3) 0.39572(3) 0.01468(8) Uani 1 1 d . . . . .
C15 C 0.59720(8) 0.61095(4) 0.35809(3) 0.01544(8) Uani 1 1 d . . . . .
C16 C 0.60428(8) 0.60088(4) 0.27162(3) 0.01617(8) Uani 1 1 d . . . . .
C17 C 0.43649(8) 0.35256(4) 0.38326(3) 0.01596(8) Uani 1 1 d . . . . .
C18 C 0.37669(8) 0.25976(4) 0.33425(4) 0.01747(9) Uani 1 1 d . . . . .
C19 C 0.31620(10) 0.17948(4) 0.29164(4) 0.02107(10) Uani 1 1 d . . . . .
C20 C 0.42833(10) 0.03876(5) 0.17190(5) 0.02600(12) Uani 1 1 d . . . . .
H20 H 0.547083 0.055582 0.211535 0.031 Uiso 1 1 calc R U . . .
C21 C 0.43916(15) 0.10956(8) 0.10943(6) 0.03816(18) Uani 1 1 d . . . . .
H21A H 0.331716 0.091347 0.064620 0.057 Uiso 1 1 calc R U . . .
H21B H 0.544966 0.107256 0.085050 0.057 Uiso 1 1 calc R U . . .
H21C H 0.447753 0.175569 0.138478 0.057 Uiso 1 1 calc R U . . .
C22 C 0.41093(15) -0.06514(7) 0.12802(7) 0.0417(2) Uani 1 1 d . . . . .
H22A H 0.406842 -0.109310 0.169320 0.063 Uiso 1 1 calc R U . . .
H22B H 0.513918 -0.068922 0.101795 0.063 Uiso 1 1 calc R U . . .
H22C H 0.300868 -0.083867 0.084768 0.063 Uiso 1 1 calc R U . . .
C23 C 0.2737(5) -0.0270(3) 0.32133(19) 0.0261(3) Uani 0.87(3) 1 d D U P A 1
H23 H 0.244560 -0.095668 0.291299 0.031 Uiso 0.87(3) 1 calc R U P A 1
C24 C 0.1399(5) -0.0181(3) 0.37847(17) 0.0331(5) Uani 0.87(3) 1 d D U P A 1
H24A H 0.167457 0.047895 0.410458 0.050 Uiso 0.87(3) 1 calc R U P A 1
H24B H 0.147873 -0.064918 0.417408 0.050 Uiso 0.87(3) 1 calc R U P A 1
H24C H 0.018729 -0.031666 0.344177 0.050 Uiso 0.87(3) 1 calc R U P A 1
C25 C 0.4619(6) -0.0092(4) 0.3756(3) 0.0361(5) Uani 0.87(3) 1 d D U P A 1
H25A H 0.547174 -0.019384 0.339612 0.054 Uiso 0.87(3) 1 calc R U P A 1
H25B H 0.464212 -0.054621 0.415980 0.054 Uiso 0.87(3) 1 calc R U P A 1
H25C H 0.494731 0.057634 0.406038 0.054 Uiso 0.87(3) 1 calc R U P A 1
C26 C 0.01955(9) 0.02597(4) 0.17951(4) 0.02151(10) Uani 1 1 d . . . . .
H26 H -0.054047 0.039299 0.222200 0.026 Uiso 1 1 calc R U . . .
C27 C -0.02062(12) 0.09034(5) 0.11410(5) 0.02986(14) Uani 1 1 d . . . . .
H27A H 0.029171 0.158565 0.138965 0.045 Uiso 1 1 calc R U . . .
H27B H -0.150245 0.080989 0.095075 0.045 Uiso 1 1 calc R U . . .
H27C H 0.033332 0.072926 0.066117 0.045 Uiso 1 1 calc R U . . .
C28 C -0.04892(11) -0.08083(5) 0.14021(6) 0.02946(14) Uani 1 1 d . . . . .
H28A H 0.015243 -0.097208 0.095800 0.044 Uiso 1 1 calc R U . . .
H28B H -0.177035 -0.092160 0.116159 0.044 Uiso 1 1 calc R U . . .
H28C H -0.028927 -0.121668 0.183456 0.044 Uiso 1 1 calc R U . . .
C29 C 0.11008(13) 0.60404(6) 0.34966(6) 0.03360(16) Uani 1 1 d . . . . .
H29A H 0.187541 0.597980 0.402760 0.040 Uiso 1 1 calc R U . . .
H29B H -0.016198 0.586637 0.354928 0.040 Uiso 1 1 calc R U . . .
C30 C 0.15325(13) 0.70690(6) 0.33131(5) 0.03236(15) Uani 1 1 d . . . . .
H30A H 0.265123 0.744359 0.369064 0.039 Uiso 1 1 calc R U . . .
H30B H 0.055140 0.740925 0.338565 0.039 Uiso 1 1 calc R U . . .
C31 C 0.17429(13) 0.69469(5) 0.24044(5) 0.03109(14) Uani 1 1 d . . . . .
H31A H 0.102220 0.733249 0.207737 0.037 Uiso 1 1 calc R U . . .
H31B H 0.301005 0.715075 0.236772 0.037 Uiso 1 1 calc R U . . .
C32 C 0.10686(13) 0.58726(5) 0.20892(5) 0.03322(16) Uani 1 1 d . . . . .
H32A H -0.022716 0.572887 0.184307 0.040 Uiso 1 1 calc R U . . .
H32B H 0.170832 0.564325 0.165693 0.040 Uiso 1 1 calc R U . . .
C33 C 0.12097(11) 0.34016(6) 0.06630(5) 0.02908(13) Uani 1 1 d . . . . .
H33A H 0.189761 0.287951 0.063672 0.035 Uiso 1 1 calc R U . . .
H33B H 0.204162 0.403475 0.072064 0.035 Uiso 1 1 calc R U . . .
C34 C -0.02315(13) 0.32471(7) -0.01145(5) 0.03348(15) Uani 1 1 d . . . . .
H34A H -0.067240 0.254749 -0.034442 0.040 Uiso 1 1 calc R U . . .
H34B H 0.019480 0.358921 -0.055420 0.040 Uiso 1 1 calc R U . . .
C35 C -0.16606(13) 0.36874(7) 0.02177(5) 0.03406(16) Uani 1 1 d . . . . .
H35A H -0.139784 0.440386 0.026358 0.041 Uiso 1 1 calc R U . . .
H35B H -0.285744 0.341772 -0.014270 0.041 Uiso 1 1 calc R U . . .
C36 C -0.15276(11) 0.33815(6) 0.10720(5) 0.03052(14) Uani 1 1 d . . . . .
H36A H -0.193197 0.384452 0.146311 0.037 Uiso 1 1 calc R U . . .
H36B H -0.226895 0.272467 0.103040 0.037 Uiso 1 1 calc R U . . .
C37 C -0.16603(13) 0.23891(7) 0.30839(6) 0.03608(17) Uani 1 1 d . . . . .
H37A H -0.128961 0.207628 0.258723 0.043 Uiso 1 1 calc R U . . .
H37B H -0.296308 0.235927 0.294541 0.043 Uiso 1 1 calc R U . . .
C38 C -0.11746(16) 0.19129(7) 0.38309(8) 0.0431(2) Uani 1 1 d . . . . .
H38A H 0.003515 0.176960 0.387614 0.052 Uiso 1 1 calc R U . . .
H38B H -0.205025 0.130495 0.381069 0.052 Uiso 1 1 calc R U . . .
C39 C -0.12417(15) 0.26896(8) 0.45480(6) 0.0405(2) Uani 1 1 d . . . . .
H39A H -0.040112 0.265583 0.506779 0.049 Uiso 1 1 calc R U . . .
H39B H -0.246229 0.262409 0.466244 0.049 Uiso 1 1 calc R U . . .
C40 C -0.06822(13) 0.36310(7) 0.42201(6) 0.03495(17) Uani 1 1 d . . . . .
H40A H -0.152755 0.406365 0.429632 0.042 Uiso 1 1 calc R U . . .
H40B H 0.052916 0.397530 0.452536 0.042 Uiso 1 1 calc R U . . .
C23X C 0.295(3) -0.0235(19) 0.3229(13) 0.0261(3) Uani 0.13(3) 1 d D U P A 2
H23X H 0.279337 -0.091533 0.293253 0.031 Uiso 0.13(3) 1 calc R U P A 2
C24X C 0.485(3) 0.0057(17) 0.3713(14) 0.029(2) Uani 0.13(3) 1 d D U P A 2
H24D H 0.562155 -0.025248 0.339982 0.044 Uiso 0.13(3) 1 calc R U P A 2
H24E H 0.492544 -0.015275 0.426268 0.044 Uiso 0.13(3) 1 calc R U P A 2
H24F H 0.524447 0.076444 0.379033 0.044 Uiso 0.13(3) 1 calc R U P A 2
C25X C 0.157(3) -0.0250(14) 0.3770(11) 0.029(2) Uani 0.13(3) 1 d D U P A 2
H25D H 0.150715 0.041785 0.398304 0.044 Uiso 0.13(3) 1 calc R U P A 2
H25E H 0.190240 -0.058334 0.424415 0.044 Uiso 0.13(3) 1 calc R U P A 2
H25F H 0.040094 -0.059522 0.343513 0.044 Uiso 0.13(3) 1 calc R U P A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0001 0.0005 '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 0.0100 0.0078 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0017 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0269 0.0229 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
C19 Si1 C20 106.86(3) . . ?
C19 Si1 C23 108.35(12) . . ?
C19 Si1 C26 109.23(3) . . ?
C19 Si1 C23X 106.8(9) . . ?
C23 Si1 C20 109.99(12) . . ?
C23 Si1 C26 107.47(12) . . ?
C26 Si1 C20 114.79(3) . . ?
C23X Si1 C20 106.4(8) . . ?
C23X Si1 C26 112.3(7) . . ?
O1 Na1 O2 97.11(2) . . ?
O1 Na1 C12 92.07(2) . . ?
O1 Na1 C13 90.80(2) . . ?
O1 Na1 C17 113.91(2) . . ?
O1 Na1 C18 142.67(2) . . ?
O2 Na1 C12 99.13(2) . . ?
O2 Na1 C13 128.81(2) . . ?
O2 Na1 C17 137.70(2) . . ?
O2 Na1 C18 112.57(2) . . ?
O3 Na1 O1 97.85(3) . . ?
O3 Na1 O2 102.15(3) . . ?
O3 Na1 C12 155.15(3) . . ?
O3 Na1 C13 126.78(3) . . ?
O3 Na1 C17 101.29(2) . . ?
O3 Na1 C18 97.45(2) . . ?
C12 Na1 C18 62.210(18) . . ?
C13 Na1 C12 29.849(17) . . ?
C13 Na1 C17 30.936(17) . . ?
C13 Na1 C18 53.162(17) . . ?
C17 Na1 C12 53.925(18) . . ?
C17 Na1 C18 29.289(16) . . ?
C29 O1 Na1 127.57(5) . . ?
C32 O1 Na1 123.16(5) . . ?
C32 O1 C29 106.83(6) . . ?
C33 O2 Na1 127.08(5) . . ?
C36 O2 Na1 119.60(5) . . ?
C36 O2 C33 109.69(6) . . ?
C37 O3 Na1 117.12(5) . . ?
C37 O3 C40 107.94(7) . . ?
C40 O3 Na1 124.41(6) . . ?
C2 C1 C1 119.21(6) . 2_666 ?
C14 C1 C1 120.69(6) . 2_666 ?
C14 C1 C2 120.09(5) . . ?
C1 C2 C17 119.86(5) . 2_666 ?
C3 C2 C1 118.60(5) . . ?
C3 C2 C17 121.55(5) . 2_666 ?
C2 C3 H3 119.0 . . ?
C4 C3 C2 122.03(5) . . ?
C4 C3 H3 119.0 . . ?
C3 C4 C5 121.42(5) . . ?
C3 C4 C15 119.97(5) . . ?
C15 C4 C5 118.60(5) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 C4 121.48(5) . . ?
C6 C5 H5 119.3 . . ?
C5 C6 H6 119.3 . . ?
C5 C6 C7 121.33(5) . . ?
C7 C6 H6 119.3 . . ?
C8 C7 C6 121.91(5) . . ?
C8 C7 C16 119.88(5) . . ?
C16 C7 C6 118.21(5) . . ?
C7 C8 H8 120.1 . . ?
C9 C8 C7 119.80(5) . . ?
C9 C8 H8 120.1 . . ?
C8 C9 H9 119.5 . . ?
C8 C9 C10 120.92(5) . . ?
C10 C9 H9 119.5 . . ?
C9 C10 H10 119.4 . . ?
C9 C10 C11 121.26(5) . . ?
C11 C10 H10 119.4 . . ?
C10 C11 C12 122.83(5) . . ?
C10 C11 C16 118.11(5) . . ?
C12 C11 C16 119.06(5) . . ?
Na1 C12 H12 85.3 . . ?
C11 C12 Na1 114.46(4) . . ?
C11 C12 H12 118.8 . . ?
C13 C12 Na1 70.46(3) . . ?
C13 C12 C11 122.41(5) . . ?
C13 C12 H12 118.8 . . ?
C12 C13 Na1 79.69(4) . . ?
C12 C13 C14 118.99(5) . . ?
C12 C13 C17 122.91(5) . . ?
C14 C13 Na1 111.44(4) . . ?
C17 C13 Na1 77.47(3) . . ?
C17 C13 C14 118.01(5) . . ?
C1 C14 C13 120.78(5) . . ?
C1 C14 C15 120.22(5) . . ?
C15 C14 C13 118.99(5) . . ?
C4 C15 C16 119.70(5) . . ?
C14 C15 C4 119.07(5) . . ?
C14 C15 C16 121.20(5) . . ?
C7 C16 C11 120.03(5) . . ?
C7 C16 C15 120.66(5) . . ?
C15 C16 C11 119.31(5) . . ?
C2 C17 Na1 117.34(4) 2_666 . ?
C13 C17 Na1 71.59(3) . . ?
C13 C17 C2 121.36(4) . 2_666 ?
C18 C17 Na1 79.91(3) . . ?
C18 C17 C2 118.83(5) . 2_666 ?
C18 C17 C13 119.76(5) . . ?
C17 C18 Na1 70.80(3) . . ?
C19 C18 Na1 106.84(5) . . ?
C19 C18 C17 176.84(7) . . ?
C18 C19 Si1 170.17(6) . . ?
Si1 C20 H20 105.8 . . ?
C21 C20 Si1 113.56(6) . . ?
C21 C20 H20 105.8 . . ?
C21 C20 C22 110.67(8) . . ?
C22 C20 Si1 114.53(6) . . ?
C22 C20 H20 105.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C23 H23 107.4 . . ?
C24 C23 Si1 112.9(2) . . ?
C24 C23 H23 107.4 . . ?
C24 C23 C25 109.1(3) . . ?
C25 C23 Si1 112.48(18) . . ?
C25 C23 H23 107.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si1 C26 H26 106.0 . . ?
C27 C26 Si1 114.71(5) . . ?
C27 C26 H26 106.0 . . ?
C27 C26 C28 109.94(6) . . ?
C28 C26 Si1 113.50(5) . . ?
C28 C26 H26 106.0 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O1 C29 H29A 110.4 . . ?
O1 C29 H29B 110.4 . . ?
O1 C29 C30 106.56(7) . . ?
H29A C29 H29B 108.6 . . ?
C30 C29 H29A 110.4 . . ?
C30 C29 H29B 110.4 . . ?
C29 C30 H30A 110.8 . . ?
C29 C30 H30B 110.8 . . ?
C29 C30 C31 104.70(6) . . ?
H30A C30 H30B 108.9 . . ?
C31 C30 H30A 110.8 . . ?
C31 C30 H30B 110.8 . . ?
C30 C31 H31A 111.0 . . ?
C30 C31 H31B 111.0 . . ?
H31A C31 H31B 109.0 . . ?
C32 C31 C30 103.95(7) . . ?
C32 C31 H31A 111.0 . . ?
C32 C31 H31B 111.0 . . ?
O1 C32 C31 105.20(6) . . ?
O1 C32 H32A 110.7 . . ?
O1 C32 H32B 110.7 . . ?
C31 C32 H32A 110.7 . . ?
C31 C32 H32B 110.7 . . ?
H32A C32 H32B 108.8 . . ?
O2 C33 H33A 110.5 . . ?
O2 C33 H33B 110.5 . . ?
O2 C33 C34 106.28(7) . . ?
H33A C33 H33B 108.7 . . ?
C34 C33 H33A 110.5 . . ?
C34 C33 H33B 110.5 . . ?
C33 C34 H34A 111.4 . . ?
C33 C34 H34B 111.4 . . ?
C33 C34 C35 101.92(7) . . ?
H34A C34 H34B 109.2 . . ?
C35 C34 H34A 111.4 . . ?
C35 C34 H34B 111.4 . . ?
C34 C35 H35A 111.4 . . ?
C34 C35 H35B 111.4 . . ?
H35A C35 H35B 109.3 . . ?
C36 C35 C34 101.63(7) . . ?
C36 C35 H35A 111.4 . . ?
C36 C35 H35B 111.4 . . ?
O2 C36 C35 105.36(7) . . ?
O2 C36 H36A 110.7 . . ?
O2 C36 H36B 110.7 . . ?
C35 C36 H36A 110.7 . . ?
C35 C36 H36B 110.7 . . ?
H36A C36 H36B 108.8 . . ?
O3 C37 H37A 111.0 . . ?
O3 C37 H37B 111.0 . . ?
O3 C37 C38 103.66(8) . . ?
H37A C37 H37B 109.0 . . ?
C38 C37 H37A 111.0 . . ?
C38 C37 H37B 111.0 . . ?
C37 C38 H38A 111.5 . . ?
C37 C38 H38B 111.5 . . ?
C37 C38 C39 101.55(8) . . ?
H38A C38 H38B 109.3 . . ?
C39 C38 H38A 111.5 . . ?
C39 C38 H38B 111.5 . . ?
C38 C39 H39A 111.2 . . ?
C38 C39 H39B 111.2 . . ?
C38 C39 C40 103.06(8) . . ?
H39A C39 H39B 109.1 . . ?
C40 C39 H39A 111.2 . . ?
C40 C39 H39B 111.2 . . ?
O3 C40 C39 106.52(7) . . ?
O3 C40 H40A 110.4 . . ?
O3 C40 H40B 110.4 . . ?
C39 C40 H40A 110.4 . . ?
C39 C40 H40B 110.4 . . ?
H40A C40 H40B 108.6 . . ?
Si1 C23X H23X 106.6 . . ?
C24X C23X Si1 110.0(12) . . ?
C24X C23X H23X 106.6 . . ?
C24X C23X C25X 114.3(17) . . ?
C25X C23X Si1 112.1(14) . . ?
C25X C23X H23X 106.6 . . ?
C23X C24X H24D 109.5 . . ?
C23X C24X H24E 109.5 . . ?
C23X C24X H24F 109.5 . . ?
H24D C24X H24E 109.5 . . ?
H24D C24X H24F 109.5 . . ?
H24E C24X H24F 109.5 . . ?
C23X C25X H25D 109.5 . . ?
C23X C25X H25E 109.5 . . ?
C23X C25X H25F 109.5 . . ?
H25D C25X H25E 109.5 . . ?
H25D C25X H25F 109.5 . . ?
H25E C25X H25F 109.5 . . ?
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
Si1 C19 1.8150(6) . ?
Si1 C20 1.8858(8) . ?
Si1 C23 1.884(2) . ?
Si1 C26 1.8846(7) . ?
Si1 C23X 1.883(16) . ?
Na1 O1 2.2468(6) . ?
Na1 O2 2.2531(6) . ?
Na1 O3 2.2340(7) . ?
Na1 C12 2.7501(7) . ?
Na1 C13 2.6342(7) . ?
Na1 C17 2.7100(6) . ?
Na1 C18 2.8254(6) . ?
O1 C29 1.4253(11) . ?
O1 C32 1.4190(10) . ?
O2 C33 1.4301(10) . ?
O2 C36 1.4301(10) . ?
O3 C37 1.4197(11) . ?
O3 C40 1.4344(11) . ?
C1 C1 1.4343(10) 2_666 ?
C1 C2 1.4242(7) . ?
C1 C14 1.4104(7) . ?
C2 C3 1.3958(8) . ?
C2 C17 1.4280(8) 2_666 ?
C3 H3 0.9500 . ?
C3 C4 1.3886(8) . ?
C4 C5 1.4265(8) . ?
C4 C15 1.4176(7) . ?
C5 H5 0.9500 . ?
C5 C6 1.3528(9) . ?
C6 H6 0.9500 . ?
C6 C7 1.4300(8) . ?
C7 C8 1.4005(8) . ?
C7 C16 1.4139(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.3825(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.3859(8) . ?
C10 H10 0.9500 . ?
C10 C11 1.4016(8) . ?
C11 C12 1.4125(8) . ?
C11 C16 1.4228(7) . ?
C12 H12 0.9500 . ?
C12 C13 1.3912(8) . ?
C13 C14 1.4425(7) . ?
C13 C17 1.4272(7) . ?
C14 C15 1.4160(7) . ?
C15 C16 1.4182(8) . ?
C17 C18 1.4039(7) . ?
C18 C19 1.2217(8) . ?
C20 H20 1.0000 . ?
C20 C21 1.5251(13) . ?
C20 C22 1.5267(10) . ?
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 H23 1.0000 . ?
C23 C24 1.529(3) . ?
C23 C25 1.532(3) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.5216(10) . ?
C26 C28 1.5267(9) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.5171(12) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C30 C31 1.5186(12) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.5093(11) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.5041(12) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.5166(13) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.5099(12) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C37 C38 1.4959(16) . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C39 1.5202(15) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.5219(15) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C23X H23X 1.0000 . ?
C23X C24X 1.504(16) . ?
C23X C25X 1.509(16) . ?
C24X H24D 0.9800 . ?
C24X H24E 0.9800 . ?
C24X H24F 0.9800 . ?
C25X H25D 0.9800 . ?
C25X H25E 0.9800 . ?
C25X H25F 0.9800 . ?
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
Na1 O1 C29 C30 167.39(6) . . . . ?
Na1 O1 C32 C31 -159.38(6) . . . . ?
Na1 O2 C33 C34 -167.13(5) . . . . ?
Na1 O2 C36 C35 144.20(6) . . . . ?
Na1 O3 C37 C38 110.38(7) . . . . ?
Na1 O3 C40 C39 -128.18(7) . . . . ?
Na1 C12 C13 C14 -108.90(5) . . . . ?
Na1 C12 C13 C17 67.64(5) . . . . ?
Na1 C13 C14 C1 88.68(5) . . . . ?
Na1 C13 C14 C15 -89.97(6) . . . . ?
Na1 C13 C17 C2 -111.35(5) . . . 2_666 ?
Na1 C13 C17 C18 66.24(5) . . . . ?
O1 C29 C30 C31 10.95(10) . . . . ?
O2 C33 C34 C35 29.71(9) . . . . ?
O3 C37 C38 C39 41.71(10) . . . . ?
C1 C1 C2 C3 -179.15(7) 2_666 . . . ?
C1 C1 C2 C17 1.19(10) 2_666 . . 2_666 ?
C1 C1 C14 C13 0.13(10) 2_666 . . . ?
C1 C1 C14 C15 178.77(6) 2_666 . . . ?
C1 C2 C3 C4 -0.41(9) . . . . ?
C1 C14 C15 C4 1.16(9) . . . . ?
C1 C14 C15 C16 -176.97(5) . . . . ?
C2 C1 C14 C13 179.65(5) . . . . ?
C2 C1 C14 C15 -1.71(9) . . . . ?
C2 C3 C4 C5 178.57(6) . . . . ?
C2 C3 C4 C15 -0.13(10) . . . . ?
C2 C17 C18 Na1 115.76(5) 2_666 . . . ?
C3 C4 C5 C6 -177.02(7) . . . . ?
C3 C4 C15 C14 -0.25(9) . . . . ?
C3 C4 C15 C16 177.92(6) . . . . ?
C4 C5 C6 C7 -1.16(11) . . . . ?
C4 C15 C16 C7 -0.56(9) . . . . ?
C4 C15 C16 C11 -179.59(5) . . . . ?
C5 C4 C15 C14 -178.98(6) . . . . ?
C5 C4 C15 C16 -0.81(9) . . . . ?
C5 C6 C7 C8 179.57(7) . . . . ?
C5 C6 C7 C16 -0.24(10) . . . . ?
C6 C7 C8 C9 179.90(6) . . . . ?
C6 C7 C16 C11 -179.88(6) . . . . ?
C6 C7 C16 C15 1.10(9) . . . . ?
C7 C8 C9 C10 -0.02(11) . . . . ?
C8 C7 C16 C11 0.30(9) . . . . ?
C8 C7 C16 C15 -178.72(6) . . . . ?
C8 C9 C10 C11 0.33(10) . . . . ?
C9 C10 C11 C12 179.03(6) . . . . ?
C9 C10 C11 C16 -0.30(9) . . . . ?
C10 C11 C12 Na1 -95.79(6) . . . . ?
C10 C11 C12 C13 -177.36(6) . . . . ?
C10 C11 C16 C7 -0.01(9) . . . . ?
C10 C11 C16 C15 179.02(5) . . . . ?
C11 C12 C13 Na1 107.16(6) . . . . ?
C11 C12 C13 C14 -1.74(9) . . . . ?
C11 C12 C13 C17 174.81(6) . . . . ?
C12 C11 C16 C7 -179.37(6) . . . . ?
C12 C11 C16 C15 -0.34(9) . . . . ?
C12 C13 C14 C1 178.55(5) . . . . ?
C12 C13 C14 C15 -0.10(8) . . . . ?
C12 C13 C17 Na1 -68.77(5) . . . . ?
C12 C13 C17 C2 179.88(6) . . . 2_666 ?
C12 C13 C17 C18 -2.53(9) . . . . ?
C13 C14 C15 C4 179.82(5) . . . . ?
C13 C14 C15 C16 1.68(9) . . . . ?
C13 C17 C18 Na1 -61.89(5) . . . . ?
C14 C1 C2 C3 1.32(9) . . . . ?
C14 C1 C2 C17 -178.34(5) . . . 2_666 ?
C14 C13 C17 Na1 107.81(5) . . . . ?
C14 C13 C17 C2 -3.54(9) . . . 2_666 ?
C14 C13 C17 C18 174.05(5) . . . . ?
C14 C15 C16 C7 177.56(6) . . . . ?
C14 C15 C16 C11 -1.46(9) . . . . ?
C15 C4 C5 C6 1.69(10) . . . . ?
C16 C7 C8 C9 -0.29(10) . . . . ?
C16 C11 C12 Na1 83.55(6) . . . . ?
C16 C11 C12 C13 1.97(9) . . . . ?
C17 C2 C3 C4 179.25(6) 2_666 . . . ?
C17 C13 C14 C1 1.84(8) . . . . ?
C17 C13 C14 C15 -176.81(5) . . . . ?
C19 Si1 C20 C21 -56.45(7) . . . . ?
C19 Si1 C20 C22 175.08(7) . . . . ?
C19 Si1 C23 C24 63.3(3) . . . . ?
C19 Si1 C23 C25 -60.7(3) . . . . ?
C19 Si1 C26 C27 58.43(6) . . . . ?
C19 Si1 C26 C28 -174.02(5) . . . . ?
C19 Si1 C23X C24X -57.3(18) . . . . ?
C19 Si1 C23X C25X 71.1(16) . . . . ?
C20 Si1 C23 C24 179.8(2) . . . . ?
C20 Si1 C23 C25 55.8(3) . . . . ?
C20 Si1 C26 C27 -61.54(6) . . . . ?
C20 Si1 C26 C28 66.02(6) . . . . ?
C20 Si1 C23X C24X 56.6(18) . . . . ?
C20 Si1 C23X C25X -175.0(13) . . . . ?
C23 Si1 C20 C21 -173.86(14) . . . . ?
C23 Si1 C20 C22 57.67(15) . . . . ?
C23 Si1 C26 C27 175.77(14) . . . . ?
C23 Si1 C26 C28 -56.67(14) . . . . ?
C26 Si1 C20 C21 64.82(7) . . . . ?
C26 Si1 C20 C22 -63.65(8) . . . . ?
C26 Si1 C23 C24 -54.6(3) . . . . ?
C26 Si1 C23 C25 -178.6(2) . . . . ?
C26 Si1 C23X C24X -177.0(14) . . . . ?
C26 Si1 C23X C25X -48.6(18) . . . . ?
C29 O1 C32 C31 37.18(9) . . . . ?
C29 C30 C31 C32 10.67(9) . . . . ?
C30 C31 C32 O1 -28.94(9) . . . . ?
C32 O1 C29 C30 -30.13(9) . . . . ?
C33 O2 C36 C35 -15.80(9) . . . . ?
C33 C34 C35 C36 -38.03(9) . . . . ?
C34 C35 C36 O2 33.65(9) . . . . ?
C36 O2 C33 C34 -9.02(8) . . . . ?
C37 O3 C40 C39 15.19(10) . . . . ?
C37 C38 C39 C40 -31.64(10) . . . . ?
C38 C39 C40 O3 11.24(10) . . . . ?
C40 O3 C37 C38 -36.03(9) . . . . ?
C23X Si1 C20 C21 -170.3(8) . . . . ?
C23X Si1 C20 C22 61.3(8) . . . . ?
C23X Si1 C26 C27 176.7(9) . . . . ?
C23X Si1 C26 C28 -55.7(9) . . . . ?
