# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_19EH064_MWS052
_database_code_depnum_ccdc_archive 'CCDC 2245605'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;

_audit_creation_date             2023-02-23T18:46:52-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C28 H63 B N3 Na O Si3'
_chemical_formula_sum            'C28 H63 B N3 Na O Si3'
_chemical_formula_weight         575.88

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   10.11080(10)
_cell_length_b                   34.6407(2)
_cell_length_c                   11.54530(10)
_cell_angle_alpha                90
_cell_angle_beta                 112.0050(10)
_cell_angle_gamma                90
_cell_volume                     3749.11(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.01(10)
_cell_measurement_reflns_used    22502
_cell_measurement_theta_min      4.32
_cell_measurement_theta_max      77.157

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_exptl_crystal_density_diffrn    1.02
_exptl_crystal_F_000             1272

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.437
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.66a (Rigaku Oxford Diffraction, 2019)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.8841
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.813
_shelx_estimated_absorpt_T_max   0.932
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.175
_oxdiff_exptl_absorpt_empirical_full_min 0.886

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      173.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.0639472
_diffrn_orient_matrix_ub_12      -0.0398144
_diffrn_orient_matrix_ub_13      -0.0081256
_diffrn_orient_matrix_ub_21      0.0721243
_diffrn_orient_matrix_ub_22      0.0172569
_diffrn_orient_matrix_ub_23      -0.0844461
_diffrn_orient_matrix_ub_31      0.1330626
_diffrn_orient_matrix_ub_32      0.0097632
_diffrn_orient_matrix_ub_33      0.1162733
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0458
_diffrn_reflns_number            36567
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         2.551
_diffrn_reflns_theta_max         77.492
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.972
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.972
_reflns_Friedel_coverage         0
_reflns_number_total             7760
_reflns_number_gt                6627
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.00   0.00   0.50    0.30    --  -18.75 109.00  24.00  114
  2  ω     23.00  88.00   0.50    0.30    --   48.55-109.00 -71.00  130
  3  ω    104.00 171.00   0.50    1.00    --  107.14 109.00  24.00  134
  4  ω     35.00 108.00   0.50    1.00    --  107.14-109.00 -71.00  146
  5  ω    -90.00   5.00   0.50    0.30    --  -18.75 -77.00 -60.00  190
  6  ω    -25.00  23.00   0.50    0.30    --   48.55 -19.00-180.00   96
  7  ω    -22.00  62.00   0.50    0.30    --   48.55 -57.00 -90.00  168
  8  ω    -25.00  23.00   0.50    0.30    --   48.55 -19.00 -90.00   96
  9  ω    -24.00  40.00   0.50    0.30    --   48.55 -38.00 150.00  128
 10  ω    -25.00  23.00   0.50    0.30    --   48.55 -19.00  30.00   96
 11  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00   0.00   54
 12  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00 -90.00   54
 13  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00  30.00   54
 14  ω     85.00 171.00   0.50    1.00    --  107.14  77.00 120.00  172
 15  ω     94.00 171.00   0.50    1.00    --  107.14  38.00  30.00  154
 16  ω     35.00 112.00   0.50    1.00    --  107.14-125.00-150.00  154
 17  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00 -60.00   54
 18  ω     35.00 106.00   0.50    1.00    --  107.14 -99.00   0.00  142
 19  ω     95.00 171.00   0.50    1.00    --  107.14 125.00 -30.00  152
 20  ω     35.00 106.00   0.50    1.00    --  107.14 -99.00  60.00  142
 21  ω     93.00 171.00   0.50    1.00    --  107.14  57.00 -90.00  156
 22  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00 120.00   54
 23  ω     35.00  62.00   0.50    1.00    --  107.14 -57.00  90.00   54
 24  ω     26.00 116.00   0.50    0.30    --   48.55  77.00-180.00  180
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.66a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0504P)²+0.9218P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7760
_refine_ls_number_parameters     438
_refine_ls_number_restraints     55
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.036
_refine_ls_wR_factor_ref         0.1027
_refine_ls_wR_factor_gt          0.0958
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.25
_refine_diff_density_min         -0.224
_refine_diff_density_rms         0.036

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_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
 C9B-C8A \\sim C9A-C8
 with sigma of 0.002
3. Rigid bond restraints
 Si1, C23, C24, C22
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Si3, C26, C28, C27
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C32, Si2, C31, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
Uanis(C8A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C4A) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C9B)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
Uanis(C7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C12A)=Sof(H12D)=Sof(H12E)=Sof(H12F)=Sof(C8A)=
 Sof(H8AA)=Sof(H8AB)=Sof(C7A)=Sof(H7AA)=Sof(H7AB)=Sof(H7AC)=Sof(N6A)=Sof(C5A)=
 Sof(H5AA)=Sof(H5AB)=Sof(N2A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)=Sof(H4AA)=
 Sof(H4AB)=Sof(H4AC)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=1-FVAR(1)
 Sof(N2)=Sof(N6)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(H4C)=
 Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=Sof(C8)=Sof(H8A)=
 Sof(H8B)=Sof(C7)=Sof(H7A)=Sof(H7B)=Sof(H7C)=Sof(C12B)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=FVAR(1)
6.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C29(H29A,H29B), C21(H21A,H21B), C5(H5A,H5B), C3(H3A,H3B),
 C8(H8A,H8B), C9A(H9AA,H9AB), C9B(H9BA,H9BB), C8A(H8AA,H8AB), C5A(H5AA,H5AB),
 C3A(H3AA,H3AB)
6.b Me refined with riding coordinates:
 C4(H4A,H4B,H4C), C1(H1A,H1B,H1C), C7(H7A,H7B,H7C), C7A(H7AA,H7AB,H7AC),
 C4A(H4AA,H4AB,H4AC), C1A(H1AA,H1AB,H1AC)
6.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C17(H17), C15(H15), C16(H16)
6.d Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C28(H28A,H28B,
 H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C26(H26A,H26B,H26C), C32(H32A,
 H32B,H32C), C20(H20A,H20B,H20C), C27(H27A,H27B,H27C), C11(H11A,H11B,H11C),
 C12B(H12A,H12B,H12C), C12A(H12D,H12E,H12F)
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.13769(4) 0.44459(2) 0.89245(3) 0.03446(10) Uani 1 1 d . U . . .
Si2 Si 0.57126(4) 0.35473(2) 0.93835(4) 0.03771(10) Uani 1 1 d . U . . .
Si3 Si 0.11432(5) 0.31072(2) 0.78824(4) 0.04183(11) Uani 1 1 d . U . . .
Na1 Na 0.30099(6) 0.36741(2) 0.52036(5) 0.03572(13) Uani 1 1 d . . . . .
O19 O 0.46877(12) 0.44990(3) 0.77224(10) 0.0475(3) Uani 1 1 d . . . . .
N10 N 0.50379(14) 0.38681(4) 0.45602(13) 0.0476(3) Uani 1 1 d . . . . .
N2 N 0.0772(6) 0.34015(19) 0.3447(6) 0.0372(8) Uani 0.732(4) 1 d . . P A 1
C25 C 0.13934(14) 0.35540(4) 0.70935(12) 0.0328(3) Uani 1 1 d . . . . .
H25A H 0.139557 0.34686 0.62759 0.039 Uiso 1 1 calc R U . . .
H25B H 0.050631 0.370505 0.690767 0.039 Uiso 1 1 calc R U . . .
C13 C 0.24633(14) 0.42181(4) 0.65604(12) 0.0316(3) Uani 1 1 d . . . . .
C29 C 0.42615(14) 0.36398(4) 0.78375(12) 0.0299(3) Uani 1 1 d . . . . .
H29A H 0.470685 0.378329 0.733625 0.036 Uiso 1 1 calc R U . . .
H29B H 0.398697 0.338444 0.743337 0.036 Uiso 1 1 calc R U . . .
C21 C 0.27230(14) 0.40783(4) 0.89317(11) 0.0308(3) Uani 1 1 d . . . . .
H21A H 0.367161 0.419966 0.933987 0.037 Uiso 1 1 calc R U . . .
H21B H 0.266642 0.386719 0.948941 0.037 Uiso 1 1 calc R U . . .
N6 N 0.3735(4) 0.30645(14) 0.4501(5) 0.0499(10) Uani 0.732(4) 1 d . . P A 1
C14 C 0.12078(17) 0.42476(4) 0.54919(13) 0.0409(3) Uani 1 1 d . . . . .
H14 H 0.048888 0.405806 0.537029 0.049 Uiso 1 1 calc R U . . .
C18 C 0.34609(16) 0.45138(4) 0.66684(14) 0.0391(3) Uani 1 1 d . . . . .
C23 C 0.14187(19) 0.45035(5) 1.05573(14) 0.0477(3) Uani 1 1 d . U . . .
H23A H 0.104101 0.426966 1.079937 0.072 Uiso 1 1 calc R U . . .
H23B H 0.083294 0.472572 1.058842 0.072 Uiso 1 1 calc R U . . .
H23C H 0.240408 0.454531 1.113506 0.072 Uiso 1 1 calc R U . . .
C22 C 0.1752(2) 0.49308(4) 0.83930(16) 0.0508(4) Uani 1 1 d . U . . .
H22A H 0.275605 0.499785 0.88468 0.076 Uiso 1 1 calc R U . . .
H22B H 0.114276 0.512555 0.855968 0.076 Uiso 1 1 calc R U . . .
H22C H 0.155325 0.492245 0.749483 0.076 Uiso 1 1 calc R U . . .
B1 B 0.27180(15) 0.38721(4) 0.76359(13) 0.0274(3) Uani 1 1 d . . . . .
C17 C 0.3232(2) 0.48062(5) 0.57820(17) 0.0544(4) Uani 1 1 d . . . . .
H17 H 0.393896 0.499799 0.588719 0.065 Uiso 1 1 calc R U . . .
C24 C -0.05126(17) 0.43219(6) 0.79282(17) 0.0572(4) Uani 1 1 d . U . . .
H24A H -0.061496 0.43093 0.705066 0.086 Uiso 1 1 calc R U . . .
H24B H -0.115245 0.452055 0.80272 0.086 Uiso 1 1 calc R U . . .
H24C H -0.075867 0.407113 0.818548 0.086 Uiso 1 1 calc R U . . .
C15 C 0.0951(2) 0.45393(5) 0.45943(16) 0.0559(4) Uani 1 1 d . . . . .
H15 H 0.008002 0.454503 0.388777 0.067 Uiso 1 1 calc R U . . .
C16 C 0.1963(2) 0.48147(5) 0.47459(17) 0.0620(5) Uani 1 1 d . . . . .
H16 H 0.180074 0.501324 0.414069 0.074 Uiso 1 1 calc R U . . .
C28 C 0.2475(2) 0.27141(5) 0.8027(2) 0.0650(5) Uani 1 1 d . U . . .
H28A H 0.234745 0.261763 0.719396 0.098 Uiso 1 1 calc R U . . .
H28B H 0.233045 0.250252 0.853072 0.098 Uiso 1 1 calc R U . . .
H28C H 0.34432 0.281695 0.843222 0.098 Uiso 1 1 calc R U . . .
C30 C 0.5164(2) 0.33323(6) 1.06269(16) 0.0626(5) Uani 1 1 d . U . . .
H30A H 0.456998 0.351732 1.085576 0.094 Uiso 1 1 calc R U . . .
H30B H 0.601596 0.3272 1.136397 0.094 Uiso 1 1 calc R U . . .
H30C H 0.461958 0.309516 1.031049 0.094 Uiso 1 1 calc R U . . .
C31 C 0.6976(2) 0.31876(6) 0.91427(19) 0.0665(5) Uani 1 1 d . U . . .
H31A H 0.646458 0.294694 0.881192 0.1 Uiso 1 1 calc R U . . .
H31B H 0.775621 0.313621 0.994215 0.1 Uiso 1 1 calc R U . . .
H31C H 0.73662 0.32921 0.854835 0.1 Uiso 1 1 calc R U . . .
C26 C 0.1079(2) 0.31926(6) 0.94651(17) 0.0637(5) Uani 1 1 d . U . . .
H26A H 0.203218 0.326275 1.005597 0.096 Uiso 1 1 calc R U . . .
H26B H 0.076069 0.295679 0.975191 0.096 Uiso 1 1 calc R U . . .
H26C H 0.041102 0.340282 0.941417 0.096 Uiso 1 1 calc R U . . .
C32 C 0.6776(2) 0.39887(6) 1.00716(19) 0.0651(5) Uani 1 1 d . U . . .
H32A H 0.72151 0.408711 0.950427 0.098 Uiso 1 1 calc R U . . .
H32B H 0.752306 0.392415 1.087802 0.098 Uiso 1 1 calc R U . . .
H32C H 0.614782 0.418663 1.019388 0.098 Uiso 1 1 calc R U . . .
C20 C 0.5633(2) 0.48209(5) 0.7988(2) 0.0635(5) Uani 1 1 d . . . . .
H20A H 0.600449 0.484938 0.732133 0.095 Uiso 1 1 calc R U . . .
H20B H 0.642641 0.477906 0.878623 0.095 Uiso 1 1 calc R U . . .
H20C H 0.511644 0.505576 0.803889 0.095 Uiso 1 1 calc R U . . .
C27 C -0.0632(2) 0.28951(6) 0.68892(19) 0.0689(5) Uani 1 1 d . U . . .
H27A H -0.139329 0.307744 0.68383 0.103 Uiso 1 1 calc R U . . .
H27B H -0.07791 0.265288 0.726335 0.103 Uiso 1 1 calc R U . . .
H27C H -0.065056 0.284433 0.604835 0.103 Uiso 1 1 calc R U . . .
C5 C 0.2639(5) 0.29430(11) 0.3317(4) 0.0532(9) Uani 0.732(4) 1 d . . P A 1
H5A H 0.279011 0.266855 0.316151 0.064 Uiso 0.732(4) 1 calc R U P A 1
H5B H 0.272485 0.30979 0.26277 0.064 Uiso 0.732(4) 1 calc R U P A 1
C4 C 0.0780(9) 0.3639(2) 0.2419(5) 0.0549(12) Uani 0.732(4) 1 d . . P A 1
H4A H 0.172811 0.363109 0.237475 0.082 Uiso 0.732(4) 1 calc R U P A 1
H4B H 0.007105 0.354089 0.163639 0.082 Uiso 0.732(4) 1 calc R U P A 1
H4C H 0.054409 0.390564 0.255065 0.082 Uiso 0.732(4) 1 calc R U P A 1
C3 C 0.1157(3) 0.29930(7) 0.3332(2) 0.0487(6) Uani 0.732(4) 1 d . . P A 1
H3A H 0.045355 0.288378 0.255123 0.058 Uiso 0.732(4) 1 calc R U P A 1
H3B H 0.109054 0.284368 0.403903 0.058 Uiso 0.732(4) 1 calc R U P A 1
C1 C -0.0627(2) 0.34069(9) 0.3539(2) 0.0502(6) Uani 0.732(4) 1 d . . P A 1
H1A H -0.060762 0.324446 0.424057 0.075 Uiso 0.732(4) 1 calc R U P A 1
H1B H -0.087049 0.367232 0.367704 0.075 Uiso 0.732(4) 1 calc R U P A 1
H1C H -0.134354 0.330757 0.276278 0.075 Uiso 0.732(4) 1 calc R U P A 1
C8 C 0.5189(4) 0.31412(9) 0.4449(4) 0.0656(10) Uani 0.732(4) 1 d D . P A 1
H8A H 0.592018 0.313212 0.530738 0.079 Uiso 0.732(4) 1 calc R U P A 1
H8B H 0.541058 0.293474 0.395733 0.079 Uiso 0.732(4) 1 calc R U P A 1
C11 C 0.4603(3) 0.41462(9) 0.3568(3) 0.1023(10) Uani 1 1 d . . . . .
H11A H 0.37865 0.404556 0.286525 0.153 Uiso 1 1 calc R U . . .
H11B H 0.539557 0.419641 0.329529 0.153 Uiso 1 1 calc R U . . .
H11C H 0.433113 0.438688 0.386676 0.153 Uiso 1 1 calc R U . . .
C7 C 0.3998(4) 0.27690(8) 0.5460(3) 0.0662(8) Uani 0.732(4) 1 d . . P A 1
H7A H 0.473589 0.285919 0.623944 0.099 Uiso 0.732(4) 1 calc R U P A 1
H7B H 0.311589 0.2718 0.559944 0.099 Uiso 0.732(4) 1 calc R U P A 1
H7C H 0.43196 0.253128 0.51868 0.099 Uiso 0.732(4) 1 calc R U P A 1
C12B C 0.6236(3) 0.39602(14) 0.5613(3) 0.0739(10) Uani 0.732(4) 1 d . . P A 1
H12A H 0.602737 0.418601 0.602784 0.111 Uiso 0.732(4) 1 calc R U P A 1
H12B H 0.703782 0.401861 0.536141 0.111 Uiso 0.732(4) 1 calc R U P A 1
H12C H 0.648347 0.374085 0.619154 0.111 Uiso 0.732(4) 1 calc R U P A 1
C9A C 0.5264(4) 0.35215(9) 0.3881(3) 0.0682(9) Uani 0.732(4) 1 d D . P A 1
H9AA H 0.453908 0.352538 0.302009 0.082 Uiso 0.732(4) 1 calc R U P A 1
H9AB H 0.621157 0.354464 0.382014 0.082 Uiso 0.732(4) 1 calc R U P A 1
C9B C 0.5917(6) 0.35297(18) 0.4661(6) 0.0476(17) Uani 0.268(4) 1 d D U P A 2
H9BA H 0.636852 0.34465 0.554354 0.057 Uiso 0.268(4) 1 calc R U P A 2
H9BB H 0.667649 0.35854 0.433857 0.057 Uiso 0.268(4) 1 calc R U P A 2
C12A C 0.6052(9) 0.4202(2) 0.5496(7) 0.0533(19) Uani 0.268(4) 1 d . . P A 2
H12D H 0.549112 0.443813 0.542869 0.08 Uiso 0.268(4) 1 calc R U P A 2
H12E H 0.686365 0.42585 0.525542 0.08 Uiso 0.268(4) 1 calc R U P A 2
H12F H 0.640128 0.410915 0.636054 0.08 Uiso 0.268(4) 1 calc R U P A 2
C8A C 0.4940(8) 0.3224(2) 0.3897(7) 0.050(2) Uani 0.268(4) 1 d D U P A 2
H8AA H 0.42627 0.33305 0.309898 0.06 Uiso 0.268(4) 1 calc R U P A 2
H8AB H 0.548152 0.300985 0.371626 0.06 Uiso 0.268(4) 1 calc R U P A 2
C7A C 0.4995(16) 0.2859(3) 0.5812(10) 0.093(3) Uani 0.268(4) 1 d . U P A 2
H7AA H 0.436122 0.279662 0.625242 0.14 Uiso 0.268(4) 1 calc R U P A 2
H7AB H 0.532169 0.262006 0.555143 0.14 Uiso 0.268(4) 1 calc R U P A 2
H7AC H 0.582051 0.300407 0.637069 0.14 Uiso 0.268(4) 1 calc R U P A 2
N6A N 0.4208(9) 0.3098(4) 0.4689(10) 0.0351(18) Uani 0.268(4) 1 d . . P A 2
C5A C 0.3071(17) 0.2874(5) 0.3799(15) 0.085(4) Uani 0.268(4) 1 d . U P A 2
H5AA H 0.348668 0.273772 0.326167 0.102 Uiso 0.268(4) 1 calc R U P A 2
H5AB H 0.279966 0.267379 0.427931 0.102 Uiso 0.268(4) 1 calc R U P A 2
N2A N 0.1131(18) 0.3324(6) 0.354(2) 0.054(4) Uani 0.268(4) 1 d . . P A 2
C3A C 0.188(2) 0.3036(4) 0.3052(13) 0.099(4) Uani 0.268(4) 1 d . U P A 2
H3AA H 0.119959 0.282575 0.266155 0.118 Uiso 0.268(4) 1 calc R U P A 2
H3AB H 0.209523 0.316373 0.237288 0.118 Uiso 0.268(4) 1 calc R U P A 2
C4A C -0.0064(17) 0.3179(5) 0.3758(13) 0.130(5) Uani 0.268(4) 1 d . U P A 2
H4AA H -0.049236 0.338591 0.40785 0.195 Uiso 0.268(4) 1 calc R U P A 2
H4AB H -0.076715 0.308024 0.297324 0.195 Uiso 0.268(4) 1 calc R U P A 2
H4AC H 0.02408 0.296907 0.437184 0.195 Uiso 0.268(4) 1 calc R U P A 2
C1A C 0.050(3) 0.3597(9) 0.246(2) 0.094(9) Uani 0.268(4) 1 d . . P A 2
H1AA H 0.126338 0.371249 0.224892 0.141 Uiso 0.268(4) 1 calc R U P A 2
H1AB H -0.015555 0.345606 0.173803 0.141 Uiso 0.268(4) 1 calc R U P A 2
H1AC H -0.002633 0.380193 0.269334 0.141 Uiso 0.268(4) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Si1 C21 1.8617(13) . ?
Si1 C23 1.8804(15) . ?
Si1 C22 1.8752(17) . ?
Si1 C24 1.8737(17) . ?
Si2 C29 1.8651(13) . ?
Si2 C30 1.8762(19) . ?
Si2 C31 1.8781(17) . ?
Si2 C32 1.8669(19) . ?
Si3 C25 1.8605(14) . ?
Si3 C28 1.878(2) . ?
Si3 C26 1.8760(18) . ?
Si3 C27 1.8802(19) . ?
Na1 N10 2.5198(14) . ?
Na1 N2 2.585(7) . ?
Na1 C13 2.6381(13) . ?
Na1 C29 2.8247(13) . ?
Na1 N6 2.470(5) . ?
Na1 C14 2.7985(15) . ?
Na1 B1 3.0106(15) . ?
Na1 N6A 2.518(12) . ?
Na1 N2A 2.46(2) . ?
O19 C18 1.3751(19) . ?
O19 C20 1.4250(19) . ?
N10 C11 1.434(3) . ?
N10 C12B 1.394(3) . ?
N10 C9A 1.497(3) . ?
N10 C9B 1.449(6) . ?
N10 C12A 1.652(7) . ?
N2 C4 1.446(9) . ?
N2 C3 1.487(6) . ?
N2 C1 1.459(6) . ?
C25 H25A 0.99 . ?
C25 H25B 0.99 . ?
C25 B1 1.6648(19) . ?
C13 C14 1.4036(19) . ?
C13 C18 1.410(2) . ?
C13 B1 1.6749(18) . ?
C29 H29A 0.99 . ?
C29 H29B 0.99 . ?
C29 B1 1.6926(18) . ?
C21 H21A 0.99 . ?
C21 H21B 0.99 . ?
C21 B1 1.6560(18) . ?
N6 C5 1.462(5) . ?
N6 C8 1.516(5) . ?
N6 C7 1.458(6) . ?
C14 H14 0.95 . ?
C14 C15 1.400(2) . ?
C18 C17 1.396(2) . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C17 H17 0.95 . ?
C17 C16 1.388(3) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C15 H15 0.95 . ?
C15 C16 1.362(3) . ?
C16 H16 0.95 . ?
C28 H28A 0.98 . ?
C28 H28B 0.98 . ?
C28 H28C 0.98 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
C31 H31A 0.98 . ?
C31 H31B 0.98 . ?
C31 H31C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C32 H32A 0.98 . ?
C32 H32B 0.98 . ?
C32 H32C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C27 H27A 0.98 . ?
C27 H27B 0.98 . ?
C27 H27C 0.98 . ?
C5 H5A 0.99 . ?
C5 H5B 0.99 . ?
C5 C3 1.515(5) . ?
C4 H4A 0.98 . ?
C4 H4B 0.98 . ?
C4 H4C 0.98 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C8 H8A 0.99 . ?
C8 H8B 0.99 . ?
C8 C9A 1.486(4) . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C12B H12A 0.98 . ?
C12B H12B 0.98 . ?
C12B H12C 0.98 . ?
C9A H9AA 0.99 . ?
C9A H9AB 0.99 . ?
C9B H9BA 0.99 . ?
C9B H9BB 0.99 . ?
C9B C8A 1.490(4) . ?
C12A H12D 0.98 . ?
C12A H12E 0.98 . ?
C12A H12F 0.98 . ?
C8A H8AA 0.99 . ?
C8A H8AB 0.99 . ?
C8A N6A 1.444(12) . ?
C7A H7AA 0.98 . ?
C7A H7AB 0.98 . ?
C7A H7AC 0.98 . ?
C7A N6A 1.492(15) . ?
N6A C5A 1.447(16) . ?
C5A H5AA 0.99 . ?
C5A H5AB 0.99 . ?
C5A C3A 1.313(18) . ?
N2A C3A 1.49(2) . ?
N2A C4A 1.41(2) . ?
N2A C1A 1.51(3) . ?
C3A H3AA 0.99 . ?
C3A H3AB 0.99 . ?
C4A H4AA 0.98 . ?
C4A H4AB 0.98 . ?
C4A H4AC 0.98 . ?
C1A H1AA 0.98 . ?
C1A H1AB 0.98 . ?
C1A H1AC 0.98 . ?

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
C21 Si1 C23 109.05(6) . . ?
C21 Si1 C22 112.15(7) . . ?
C21 Si1 C24 114.93(7) . . ?
C22 Si1 C23 107.55(7) . . ?
C24 Si1 C23 105.94(8) . . ?
C24 Si1 C22 106.80(9) . . ?
C29 Si2 C30 116.64(7) . . ?
C29 Si2 C31 107.88(7) . . ?
C29 Si2 C32 112.81(7) . . ?
C30 Si2 C31 105.21(10) . . ?
C32 Si2 C30 106.73(10) . . ?
C32 Si2 C31 106.93(10) . . ?
C25 Si3 C28 114.97(8) . . ?
C25 Si3 C26 113.97(8) . . ?
C25 Si3 C27 107.49(8) . . ?
C28 Si3 C27 105.07(11) . . ?
C26 Si3 C28 108.24(10) . . ?
C26 Si3 C27 106.38(9) . . ?
N10 Na1 N2 115.83(15) . . ?
N10 Na1 C13 111.05(5) . . ?
N10 Na1 C29 104.05(4) . . ?
N10 Na1 C14 118.93(5) . . ?
N10 Na1 B1 126.10(5) . . ?
N2 Na1 C13 114.22(12) . . ?
N2 Na1 C29 137.44(16) . . ?
N2 Na1 C14 86.29(11) . . ?
N2 Na1 B1 116.88(14) . . ?
C13 Na1 C29 59.99(4) . . ?
C13 Na1 C14 29.74(4) . . ?
C13 Na1 B1 33.68(4) . . ?
C29 Na1 B1 33.53(4) . . ?
N6 Na1 N10 75.91(10) . . ?
N6 Na1 N2 73.16(14) . . ?
N6 Na1 C13 163.71(13) . . ?
N6 Na1 C29 104.44(13) . . ?
N6 Na1 C14 158.85(9) . . ?
N6 Na1 B1 130.25(13) . . ?
C14 Na1 C29 87.18(4) . . ?
C14 Na1 B1 55.36(4) . . ?
N6A Na1 N10 68.0(2) . . ?
N6A Na1 C13 158.8(2) . . ?
N6A Na1 C29 99.2(2) . . ?
N6A Na1 C14 169.3(2) . . ?
N6A Na1 B1 128.6(2) . . ?
N2A Na1 N10 112.3(5) . . ?
N2A Na1 C13 122.9(4) . . ?
N2A Na1 C29 136.3(5) . . ?
N2A Na1 C14 95.5(3) . . ?
N2A Na1 B1 121.6(5) . . ?
N2A Na1 N6A 74.0(4) . . ?
C18 O19 C20 118.10(13) . . ?
C11 N10 Na1 112.02(14) . . ?
C11 N10 C9A 100.5(2) . . ?
C11 N10 C9B 127.1(3) . . ?
C11 N10 C12A 88.9(3) . . ?
C12B N10 Na1 109.93(15) . . ?
C12B N10 C11 116.7(2) . . ?
C12B N10 C9A 112.8(2) . . ?
C9A N10 Na1 103.96(13) . . ?
C9B N10 Na1 107.6(3) . . ?
C9B N10 C12A 107.6(4) . . ?
C12A N10 Na1 111.6(3) . . ?
C4 N2 Na1 99.4(5) . . ?
C4 N2 C3 112.7(5) . . ?
C4 N2 C1 110.9(4) . . ?
C3 N2 Na1 103.7(2) . . ?
C1 N2 Na1 121.7(4) . . ?
C1 N2 C3 108.2(5) . . ?
Si3 C25 H25A 105.5 . . ?
Si3 C25 H25B 105.5 . . ?
H25A C25 H25B 106.1 . . ?
B1 C25 Si3 127.17(9) . . ?
B1 C25 H25A 105.5 . . ?
B1 C25 H25B 105.5 . . ?
C14 C13 Na1 81.47(8) . . ?
C14 C13 C18 113.98(12) . . ?
C14 C13 B1 122.74(12) . . ?
C18 C13 Na1 105.62(9) . . ?
C18 C13 B1 123.24(11) . . ?
B1 C13 Na1 85.45(7) . . ?
Si2 C29 Na1 155.78(6) . . ?
Si2 C29 H29A 106.2 . . ?
Si2 C29 H29B 106.2 . . ?
Na1 C29 H29A 57.9 . . ?
Na1 C29 H29B 66.2 . . ?
H29A C29 H29B 106.4 . . ?
B1 C29 Si2 124.57(9) . . ?
B1 C29 Na1 79.27(6) . . ?
B1 C29 H29A 106.2 . . ?
B1 C29 H29B 106.2 . . ?
Si1 C21 H21A 106.7 . . ?
Si1 C21 H21B 106.7 . . ?
H21A C21 H21B 106.6 . . ?
B1 C21 Si1 122.43(8) . . ?
B1 C21 H21A 106.7 . . ?
B1 C21 H21B 106.7 . . ?
C5 N6 Na1 109.8(3) . . ?
C5 N6 C8 114.8(4) . . ?
C8 N6 Na1 105.9(2) . . ?
C7 N6 Na1 110.0(3) . . ?
C7 N6 C5 111.5(3) . . ?
C7 N6 C8 104.4(4) . . ?
Na1 C14 H14 89.3 . . ?
C13 C14 Na1 68.79(8) . . ?
C13 C14 H14 118 . . ?
C15 C14 Na1 111.89(11) . . ?
C15 C14 C13 123.98(16) . . ?
C15 C14 H14 118 . . ?
O19 C18 C13 115.44(12) . . ?
O19 C18 C17 121.50(14) . . ?
C17 C18 C13 123.06(15) . . ?
Si1 C23 H23A 109.5 . . ?
Si1 C23 H23B 109.5 . . ?
Si1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 B1 Na1 81.06(7) . . ?
C25 B1 C13 108.44(10) . . ?
C25 B1 C29 107.90(10) . . ?
C13 B1 Na1 60.87(6) . . ?
C13 B1 C29 108.66(10) . . ?
C29 B1 Na1 67.20(6) . . ?
C21 B1 Na1 166.57(9) . . ?
C21 B1 C25 110.79(10) . . ?
C21 B1 C13 107.98(10) . . ?
C21 B1 C29 112.97(10) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 C18 119.53(17) . . ?
C16 C17 H17 120.2 . . ?
Si1 C24 H24A 109.5 . . ?
Si1 C24 H24B 109.5 . . ?
Si1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C14 C15 H15 120.4 . . ?
C16 C15 C14 119.22(16) . . ?
C16 C15 H15 120.4 . . ?
C17 C16 H16 119.9 . . ?
C15 C16 C17 120.22(15) . . ?
C15 C16 H16 119.9 . . ?
Si3 C28 H28A 109.5 . . ?
Si3 C28 H28B 109.5 . . ?
Si3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C30 H30A 109.5 . . ?
Si2 C30 H30B 109.5 . . ?
Si2 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
Si2 C31 H31A 109.5 . . ?
Si2 C31 H31B 109.5 . . ?
Si2 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
Si3 C26 H26A 109.5 . . ?
Si3 C26 H26B 109.5 . . ?
Si3 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
Si2 C32 H32A 109.5 . . ?
Si2 C32 H32B 109.5 . . ?
Si2 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O19 C20 H20A 109.5 . . ?
O19 C20 H20B 109.5 . . ?
O19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si3 C27 H27A 109.5 . . ?
Si3 C27 H27B 109.5 . . ?
Si3 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N6 C5 H5A 109.4 . . ?
N6 C5 H5B 109.4 . . ?
N6 C5 C3 111.3(3) . . ?
H5A C5 H5B 108 . . ?
C3 C5 H5A 109.4 . . ?
C3 C5 H5B 109.4 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
N2 C3 C5 113.7(3) . . ?
N2 C3 H3A 108.8 . . ?
N2 C3 H3B 108.8 . . ?
C5 C3 H3A 108.8 . . ?
C5 C3 H3B 108.8 . . ?
H3A C3 H3B 107.7 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N6 C8 H8A 109.1 . . ?
N6 C8 H8B 109.1 . . ?
H8A C8 H8B 107.8 . . ?
C9A C8 N6 112.5(3) . . ?
C9A C8 H8A 109.1 . . ?
C9A C8 H8B 109.1 . . ?
N10 C11 H11A 109.5 . . ?
N10 C11 H11B 109.5 . . ?
N10 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N6 C7 H7A 109.5 . . ?
N6 C7 H7B 109.5 . . ?
N6 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N10 C12B H12A 109.5 . . ?
N10 C12B H12B 109.5 . . ?
N10 C12B H12C 109.5 . . ?
H12A C12B H12B 109.5 . . ?
H12A C12B H12C 109.5 . . ?
H12B C12B H12C 109.5 . . ?
N10 C9A H9AA 108.3 . . ?
N10 C9A H9AB 108.3 . . ?
C8 C9A N10 115.9(2) . . ?
C8 C9A H9AA 108.3 . . ?
C8 C9A H9AB 108.3 . . ?
H9AA C9A H9AB 107.4 . . ?
N10 C9B H9BA 110.5 . . ?
N10 C9B H9BB 110.5 . . ?
N10 C9B C8A 106.0(5) . . ?
H9BA C9B H9BB 108.7 . . ?
C8A C9B H9BA 110.5 . . ?
C8A C9B H9BB 110.5 . . ?
N10 C12A H12D 109.5 . . ?
N10 C12A H12E 109.5 . . ?
N10 C12A H12F 109.5 . . ?
H12D C12A H12E 109.5 . . ?
H12D C12A H12F 109.5 . . ?
H12E C12A H12F 109.5 . . ?
C9B C8A H8AA 111.2 . . ?
C9B C8A H8AB 111.2 . . ?
H8AA C8A H8AB 109.1 . . ?
N6A C8A C9B 102.9(7) . . ?
N6A C8A H8AA 111.2 . . ?
N6A C8A H8AB 111.2 . . ?
H7AA C7A H7AB 109.5 . . ?
H7AA C7A H7AC 109.5 . . ?
H7AB C7A H7AC 109.5 . . ?
N6A C7A H7AA 109.5 . . ?
N6A C7A H7AB 109.5 . . ?
N6A C7A H7AC 109.5 . . ?
C8A N6A Na1 108.4(7) . . ?
C8A N6A C7A 119.0(9) . . ?
C8A N6A C5A 99.9(10) . . ?
C7A N6A Na1 112.4(7) . . ?
C5A N6A Na1 105.6(8) . . ?
C5A N6A C7A 110.1(11) . . ?
N6A C5A H5AA 106.9 . . ?
N6A C5A H5AB 106.9 . . ?
H5AA C5A H5AB 106.7 . . ?
C3A C5A N6A 121.7(14) . . ?
C3A C5A H5AA 106.9 . . ?
C3A C5A H5AB 106.9 . . ?
C3A N2A Na1 105.7(10) . . ?
C3A N2A C1A 103.0(18) . . ?
C4A N2A Na1 120.1(13) . . ?
C4A N2A C3A 114.9(17) . . ?
C4A N2A C1A 104.1(15) . . ?
C1A N2A Na1 107.5(16) . . ?
C5A C3A N2A 120.5(13) . . ?
C5A C3A H3AA 107.2 . . ?
C5A C3A H3AB 107.2 . . ?
N2A C3A H3AA 107.2 . . ?
N2A C3A H3AB 107.2 . . ?
H3AA C3A H3AB 106.8 . . ?
N2A C4A H4AA 109.5 . . ?
N2A C4A H4AB 109.5 . . ?
N2A C4A H4AC 109.5 . . ?
H4AA C4A H4AB 109.5 . . ?
H4AA C4A H4AC 109.5 . . ?
H4AB C4A H4AC 109.5 . . ?
N2A C1A H1AA 109.5 . . ?
N2A C1A H1AB 109.5 . . ?
N2A C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si1 C21 B1 Na1 77.4(4) . . . . ?
Si1 C21 B1 C25 -73.59(13) . . . . ?
Si1 C21 B1 C13 45.02(14) . . . . ?
Si1 C21 B1 C29 165.22(9) . . . . ?
Si2 C29 B1 Na1 175.30(10) . . . . ?
Si2 C29 B1 C25 -112.94(11) . . . . ?
Si2 C29 B1 C13 129.68(10) . . . . ?
Si2 C29 B1 C21 9.88(15) . . . . ?
Si3 C25 B1 Na1 123.97(10) . . . . ?
Si3 C25 B1 C13 179.09(9) . . . . ?
Si3 C25 B1 C29 61.56(14) . . . . ?
Si3 C25 B1 C21 -62.58(14) . . . . ?
Na1 N10 C9A C8 -41.5(3) . . . . ?
Na1 N10 C9B C8A 54.6(5) . . . . ?
Na1 N2 C3 C5 -45.5(4) . . . . ?
Na1 C13 C14 C15 -102.76(16) . . . . ?
Na1 C13 C18 O19 -94.16(12) . . . . ?
Na1 C13 C18 C17 86.47(16) . . . . ?
Na1 C13 B1 C25 -68.08(9) . . . . ?
Na1 C13 B1 C29 48.96(9) . . . . ?
Na1 C13 B1 C21 171.82(9) . . . . ?
Na1 C29 B1 C25 71.76(8) . . . . ?
Na1 C29 B1 C13 -45.62(8) . . . . ?
Na1 C29 B1 C21 -165.42(10) . . . . ?
Na1 N6 C5 C3 -43.0(4) . . . . ?
Na1 N6 C8 C9A -43.2(4) . . . . ?
Na1 C14 C15 C16 -78.53(19) . . . . ?
Na1 N6A C5A C3A 27.6(19) . . . . ?
Na1 N2A C3A C5A 34(2) . . . . ?
O19 C18 C17 C16 -178.54(16) . . . . ?
N10 C9B C8A N6A -77.0(8) . . . . ?
C13 C14 C15 C16 0.0(3) . . . . ?
C13 C18 C17 C16 0.8(3) . . . . ?
N6 C5 C3 N2 64.1(5) . . . . ?
N6 C8 C9A N10 62.2(5) . . . . ?
C14 C13 C18 O19 178.37(12) . . . . ?
C14 C13 C18 C17 -1.0(2) . . . . ?
C14 C13 B1 Na1 76.82(12) . . . . ?
C14 C13 B1 C25 8.74(17) . . . . ?
C14 C13 B1 C29 125.78(13) . . . . ?
C14 C13 B1 C21 -111.36(13) . . . . ?
C14 C15 C16 C17 -0.2(3) . . . . ?
C18 C13 C14 Na1 103.38(11) . . . . ?
C18 C13 C14 C15 0.6(2) . . . . ?
C18 C13 B1 Na1 -105.72(13) . . . . ?
C18 C13 B1 C25 -173.79(12) . . . . ?
C18 C13 B1 C29 -56.75(15) . . . . ?
C18 C13 B1 C21 66.11(15) . . . . ?
C18 C17 C16 C15 -0.1(3) . . . . ?
C23 Si1 C21 B1 164.22(11) . . . . ?
C22 Si1 C21 B1 -76.77(12) . . . . ?
B1 C13 C14 Na1 -78.94(11) . . . . ?
B1 C13 C14 C15 178.30(14) . . . . ?
B1 C13 C18 O19 0.70(19) . . . . ?
B1 C13 C18 C17 -178.66(14) . . . . ?
C24 Si1 C21 B1 45.47(14) . . . . ?
C28 Si3 C25 B1 -69.10(14) . . . . ?
C30 Si2 C29 Na1 -142.22(16) . . . . ?
C30 Si2 C29 B1 49.08(14) . . . . ?
C31 Si2 C29 Na1 -24.17(19) . . . . ?
C31 Si2 C29 B1 167.13(12) . . . . ?
C26 Si3 C25 B1 56.70(14) . . . . ?
C32 Si2 C29 Na1 93.70(17) . . . . ?
C32 Si2 C29 B1 -74.99(13) . . . . ?
C20 O19 C18 C13 -170.18(15) . . . . ?
C20 O19 C18 C17 9.2(2) . . . . ?
C27 Si3 C25 B1 174.33(13) . . . . ?
C5 N6 C8 C9A 78.1(5) . . . . ?
C4 N2 C3 C5 61.1(6) . . . . ?
C1 N2 C3 C5 -176.0(3) . . . . ?
C8 N6 C5 C3 -162.2(4) . . . . ?
C11 N10 C9A C8 -157.6(3) . . . . ?
C11 N10 C9B C8A -82.6(6) . . . . ?
C7 N6 C5 C3 79.2(4) . . . . ?
C7 N6 C8 C9A -159.4(3) . . . . ?
C12B N10 C9A C8 77.5(4) . . . . ?
C9B C8A N6A Na1 57.1(7) . . . . ?
C9B C8A N6A C7A -73.0(12) . . . . ?
C9B C8A N6A C5A 167.3(9) . . . . ?
C12A N10 C9B C8A 175.0(5) . . . . ?
C8A N6A C5A C3A -84.8(19) . . . . ?
C7A N6A C5A C3A 149.2(17) . . . . ?
N6A C5A C3A N2A -46(3) . . . . ?
C4A N2A C3A C5A -101(2) . . . . ?
C1A N2A C3A C5A 146(2) . . . . ?

#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL FILE                                           #
#----------------------------------------------------------------------------#


# END of CIF
####################################################################### 
# 
# 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_20EH110_MWS137
_database_code_depnum_ccdc_archive 'CCDC 2245609'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;

_audit_creation_date             2022-08-05T17:14:18-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C21 H55 B N3 Na Si3'
_chemical_formula_sum            'C21 H55 B N3 Na Si3'
_chemical_formula_weight         467.75

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.50294(10)
_cell_length_b                   16.73895(15)
_cell_length_c                   15.65536(13)
_cell_angle_alpha                90
_cell_angle_beta                 98.9971(8)
_cell_angle_gamma                90
_cell_volume                     3236.14(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.00(10)
_cell_measurement_reflns_used    24241
_cell_measurement_theta_min      2.632
_cell_measurement_theta_max      76.838

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       plate
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.018
_exptl_crystal_density_diffrn    0.96
_exptl_crystal_F_000             1040

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.549
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.41.72a (Rigaku Oxford Diffraction, 2020)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.27347
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.737
_shelx_estimated_absorpt_T_max   0.973

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      173.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0313289
_diffrn_orient_matrix_ub_12      0.0112019
_diffrn_orient_matrix_ub_13      0.0905664
_diffrn_orient_matrix_ub_21      0.0039464
_diffrn_orient_matrix_ub_22      -0.09117
_diffrn_orient_matrix_ub_23      0.0136217
_diffrn_orient_matrix_ub_31      0.1206692
_diffrn_orient_matrix_ub_32      0.0059902
_diffrn_orient_matrix_ub_33      0.0392438
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_number            37617
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         3.892
_diffrn_reflns_theta_max         76.888
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_reflns_Friedel_coverage         0
_reflns_number_total             6649
_reflns_number_gt                5757
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0765P)²+1.3822P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6649
_refine_ls_number_parameters     280
_refine_ls_number_restraints     25
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0511
_refine_ls_wR_factor_ref         0.1492
_refine_ls_wR_factor_gt          0.1415
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.07
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.612
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.047

#----------------------------------------------------------------------------#
#                   SQUEEZE                                                  #
#----------------------------------------------------------------------------#

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.237 0.052 0.734 18.4 0.3 ?
2 0.263 0.552 0.766 18.4 0.3 ?
3 0.737 0.448 0.234 18.4 0.3 ?
4 0.763 -0.052 0.266 18.4 0.3 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Si3 Si 0.53317(4) 0.44296(3) 0.83635(3) 0.04268(15) Uani 1 1 d . U . . .
Si1 Si 0.25841(4) 0.30039(4) 0.62845(3) 0.04515(15) Uani 1 1 d . U . . .
Si2 Si 0.56601(5) 0.14196(3) 0.77356(4) 0.04830(16) Uani 1 1 d . U . . .
Na1 Na 0.60194(6) 0.26514(4) 0.58363(4) 0.03967(18) Uani 1 1 d . . . . .
N1 N 0.57993(15) 0.16123(11) 0.46381(11) 0.0525(4) Uani 1 1 d . . . . .
N3 N 0.79067(14) 0.32434(12) 0.60499(13) 0.0563(4) Uani 1 1 d . U . . .
N2 N 0.62158(16) 0.33809(12) 0.44582(13) 0.0573(5) Uani 1 1 d . . . . .
C9 C 0.49779(15) 0.39785(11) 0.72664(12) 0.0395(4) Uani 1 1 d . . . . .
H9A H 0.431902 0.424067 0.695794 0.047 Uiso 1 1 calc R U . . .
H9B H 0.557515 0.407694 0.693245 0.047 Uiso 1 1 calc R U . . .
C5 C 0.56604(15) 0.24494(11) 0.73726(12) 0.0396(4) Uani 1 1 d . . . . .
C4 C 0.35238(15) 0.27824(12) 0.73072(12) 0.0441(4) Uani 1 1 d . . . . .
H4A H 0.32555 0.306275 0.778875 0.053 Uiso 1 1 calc R U . . .
H4B H 0.34957 0.220193 0.742287 0.053 Uiso 1 1 calc R U . . .
B1 B 0.47680(16) 0.30319(12) 0.73121(12) 0.0343(4) Uani 1 1 d . . . . .
C8 C 0.5272(2) 0.12915(17) 0.88400(15) 0.0660(6) Uani 1 1 d . U . . .
H8A H 0.577511 0.159347 0.92637 0.099 Uiso 1 1 calc R U . . .
H8B H 0.530538 0.07241 0.89962 0.099 Uiso 1 1 calc R U . . .
H8C H 0.453414 0.149006 0.883578 0.099 Uiso 1 1 calc R U . . .
C13 C 0.4677(2) 0.13430(17) 0.43906(18) 0.0675(7) Uani 1 1 d . . . . .
H13A H 0.444203 0.106064 0.487732 0.101 Uiso 1 1 calc R U . . .
H13B H 0.463158 0.098217 0.389325 0.101 Uiso 1 1 calc R U . . .
H13C H 0.420749 0.18064 0.423573 0.101 Uiso 1 1 calc R U . . .
C10 C 0.6733(2) 0.41647(17) 0.88711(16) 0.0653(6) Uani 1 1 d . U . . .
H10A H 0.681076 0.35821 0.889205 0.098 Uiso 1 1 calc R U . . .
H10B H 0.687474 0.43807 0.945977 0.098 Uiso 1 1 calc R U . . .
H10C H 0.725152 0.439159 0.852883 0.098 Uiso 1 1 calc R U . . .
C12 C 0.4384(2) 0.40894(19) 0.90964(17) 0.0774(8) Uani 1 1 d . U . . .
H12A H 0.364403 0.425074 0.885696 0.116 Uiso 1 1 calc R U . . .
H12B H 0.459039 0.433215 0.966806 0.116 Uiso 1 1 calc R U . . .
H12C H 0.441814 0.350628 0.914983 0.116 Uiso 1 1 calc R U . . .
C19 C 0.7864(2) 0.38595(17) 0.5344(2) 0.0739(6) Uani 1 1 d . U . . .
H19A H 0.746331 0.433195 0.550611 0.089 Uiso 1 1 calc R U . . .
H19B H 0.861141 0.403258 0.530452 0.089 Uiso 1 1 calc R U . . .
C11 C 0.5253(3) 0.55399(14) 0.82757(19) 0.0720(7) Uani 1 1 d . U . . .
H11A H 0.568718 0.572252 0.784342 0.108 Uiso 1 1 calc R U . . .
H11B H 0.553393 0.577897 0.883754 0.108 Uiso 1 1 calc R U . . .
H11C H 0.449767 0.570174 0.809987 0.108 Uiso 1 1 calc R U . . .
C15 C 0.6217(2) 0.19708(17) 0.39113(16) 0.0693(7) Uani 1 1 d . . . . .
H15A H 0.598923 0.164194 0.33888 0.083 Uiso 1 1 calc R U . . .
H15B H 0.701788 0.196755 0.403148 0.083 Uiso 1 1 calc R U . . .
C1 C 0.1789(2) 0.39322(16) 0.63936(18) 0.0690(6) Uani 1 1 d . U . . .
H1A H 0.13365 0.385598 0.684481 0.104 Uiso 1 1 calc R U . . .
H1B H 0.132702 0.40482 0.58423 0.104 Uiso 1 1 calc R U . . .
H1C H 0.228627 0.437969 0.655099 0.104 Uiso 1 1 calc R U . . .
C16 C 0.5835(3) 0.28075(18) 0.37331(15) 0.0723(7) Uani 1 1 d . . . . .
H16A H 0.503329 0.280993 0.362165 0.087 Uiso 1 1 calc R U . . .
H16B H 0.609217 0.29976 0.320188 0.087 Uiso 1 1 calc R U . . .
C3 C 0.3328(2) 0.3147(2) 0.53556(15) 0.0830(9) Uani 1 1 d . U . . .
H3A H 0.380648 0.361138 0.546385 0.125 Uiso 1 1 calc R U . . .
H3B H 0.280827 0.323435 0.482688 0.125 Uiso 1 1 calc R U . . .
H3C H 0.376029 0.266948 0.528669 0.125 Uiso 1 1 calc R U . . .
C2 C 0.1628(2) 0.21496(18) 0.6010(2) 0.0780(7) Uani 1 1 d . U . . .
H2A H 0.204121 0.166104 0.594804 0.117 Uiso 1 1 calc R U . . .
H2B H 0.115018 0.226234 0.546581 0.117 Uiso 1 1 calc R U . . .
H2C H 0.119277 0.207755 0.647352 0.117 Uiso 1 1 calc R U . . .
C17 C 0.5554(2) 0.41094(16) 0.4339(2) 0.0772(8) Uani 1 1 d . . . . .
H17A H 0.478643 0.396712 0.429093 0.116 Uiso 1 1 calc R U . . .
H17B H 0.567963 0.438278 0.381002 0.116 Uiso 1 1 calc R U . . .
H17C H 0.575388 0.446421 0.483612 0.116 Uiso 1 1 calc R U . . .
C18 C 0.7350(2) 0.35827(18) 0.44920(19) 0.0731(7) Uani 1 1 d . U . . .
H18A H 0.74146 0.400561 0.406087 0.088 Uiso 1 1 calc R U . . .
H18B H 0.774328 0.310641 0.432997 0.088 Uiso 1 1 calc R U . . .
C21 C 0.8203(2) 0.3632(2) 0.6881(2) 0.0824(8) Uani 1 1 d . U . . .
H21A H 0.765491 0.403252 0.695911 0.124 Uiso 1 1 calc R U . . .
H21B H 0.890826 0.389239 0.690337 0.124 Uiso 1 1 calc R U . . .
H21C H 0.824493 0.32323 0.734306 0.124 Uiso 1 1 calc R U . . .
C6 C 0.4722(3) 0.07290(16) 0.7033(2) 0.0829(8) Uani 1 1 d . U . . .
H6A H 0.397158 0.089985 0.70295 0.124 Uiso 1 1 calc R U . . .
H6B H 0.481522 0.018356 0.725957 0.124 Uiso 1 1 calc R U . . .
H6C H 0.488874 0.074278 0.644166 0.124 Uiso 1 1 calc R U . . .
C14 C 0.6473(2) 0.09041(17) 0.4930(2) 0.0760(7) Uani 1 1 d . . . . .
H14A H 0.721802 0.107493 0.513819 0.114 Uiso 1 1 calc R U . . .
H14B H 0.646782 0.053266 0.444568 0.114 Uiso 1 1 calc R U . . .
H14C H 0.617831 0.063704 0.539964 0.114 Uiso 1 1 calc R U . . .
C7 C 0.7076(3) 0.09963(19) 0.7804(2) 0.0905(9) Uani 1 1 d . U . . .
H7A H 0.724394 0.091503 0.721977 0.136 Uiso 1 1 calc R U . . .
H7B H 0.711849 0.048422 0.811129 0.136 Uiso 1 1 calc R U . . .
H7C H 0.759887 0.137076 0.811799 0.136 Uiso 1 1 calc R U . . .
C20 C 0.8672(3) 0.2628(2) 0.5944(3) 0.1049(12) Uani 1 1 d . U . . .
H20A H 0.871969 0.225207 0.642775 0.157 Uiso 1 1 calc R U . . .
H20B H 0.938415 0.286828 0.593097 0.157 Uiso 1 1 calc R U . . .
H20C H 0.843504 0.234405 0.53998 0.157 Uiso 1 1 calc R U . . .
H5 H 0.6375(19) 0.2668(13) 0.7411(14) 0.048(6) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Si3 C9 1.8651(19) . ?
Si3 C10 1.861(2) . ?
Si3 C12 1.863(2) . ?
Si3 C11 1.865(2) . ?
Si1 C4 1.869(2) . ?
Si1 C1 1.867(3) . ?
Si1 C3 1.860(2) . ?
Si1 C2 1.870(3) . ?
Si2 C5 1.8149(19) . ?
Si2 C8 1.880(2) . ?
Si2 C6 1.876(3) . ?
Si2 C7 1.894(3) . ?
Na1 N1 2.5413(18) . ?
Na1 N3 2.5328(19) . ?
Na1 N2 2.5242(19) . ?
Na1 C5 2.5373(19) . ?
Na1 B1 3.053(2) . ?
Na1 H5 2.44(2) . ?
N1 C13 1.467(3) . ?
N1 C15 1.454(3) . ?
N1 C14 1.484(3) . ?
N3 C19 1.507(3) . ?
N3 C21 1.450(3) . ?
N3 C20 1.433(3) . ?
N2 C16 1.506(3) . ?
N2 C17 1.469(3) . ?
N2 C18 1.451(3) . ?
C9 H9A 0.99 . ?
C9 H9B 0.99 . ?
C9 B1 1.609(3) . ?
C5 B1 1.474(3) . ?
C5 H5 0.96(2) . ?
C4 H4A 0.99 . ?
C4 H4B 0.99 . ?
C4 B1 1.610(3) . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C19 H19A 0.99 . ?
C19 H19B 0.99 . ?
C19 C18 1.462(4) . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C15 C16 1.492(4) . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C3 H3A 0.98 . ?
C3 H3B 0.98 . ?
C3 H3C 0.98 . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C6 H6A 0.98 . ?
C6 H6B 0.98 . ?
C6 H6C 0.98 . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?

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 Si3 C11 109.48(11) . . ?
C10 Si3 C9 111.63(10) . . ?
C10 Si3 C12 108.14(14) . . ?
C10 Si3 C11 107.71(13) . . ?
C12 Si3 C9 111.18(10) . . ?
C12 Si3 C11 108.60(14) . . ?
C4 Si1 C2 109.78(12) . . ?
C1 Si1 C4 111.05(11) . . ?
C1 Si1 C2 109.10(14) . . ?
C3 Si1 C4 111.78(10) . . ?
C3 Si1 C1 107.64(15) . . ?
C3 Si1 C2 107.37(15) . . ?
C5 Si2 C8 114.15(11) . . ?
C5 Si2 C6 115.61(12) . . ?
C5 Si2 C7 109.10(12) . . ?
C8 Si2 C7 106.15(14) . . ?
C6 Si2 C8 103.98(14) . . ?
C6 Si2 C7 107.22(16) . . ?
N1 Na1 B1 133.80(6) . . ?
N1 Na1 H5 137.4(5) . . ?
N3 Na1 N1 110.88(6) . . ?
N3 Na1 C5 103.08(7) . . ?
N3 Na1 B1 113.30(6) . . ?
N3 Na1 H5 81.0(6) . . ?
N2 Na1 N1 73.38(7) . . ?
N2 Na1 N3 73.17(7) . . ?
N2 Na1 C5 158.42(7) . . ?
N2 Na1 B1 132.51(6) . . ?
N2 Na1 H5 146.4(5) . . ?
C5 Na1 N1 126.42(7) . . ?
C5 Na1 B1 28.72(6) . . ?
C5 Na1 H5 22.1(5) . . ?
B1 Na1 H5 42.7(5) . . ?
C13 N1 Na1 113.20(14) . . ?
C13 N1 C14 108.0(2) . . ?
C15 N1 Na1 106.53(14) . . ?
C15 N1 C13 111.4(2) . . ?
C15 N1 C14 108.4(2) . . ?
C14 N1 Na1 109.18(15) . . ?
C19 N3 Na1 104.19(14) . . ?
C21 N3 Na1 113.30(15) . . ?
C21 N3 C19 109.1(2) . . ?
C20 N3 Na1 109.19(18) . . ?
C20 N3 C19 110.8(3) . . ?
C20 N3 C21 110.2(3) . . ?
C16 N2 Na1 105.93(14) . . ?
C17 N2 Na1 112.46(15) . . ?
C17 N2 C16 109.1(2) . . ?
C18 N2 Na1 107.85(15) . . ?
C18 N2 C16 111.6(2) . . ?
C18 N2 C17 109.8(2) . . ?
Si3 C9 H9A 109.2 . . ?
Si3 C9 H9B 109.2 . . ?
H9A C9 H9B 107.9 . . ?
B1 C9 Si3 112.00(12) . . ?
B1 C9 H9A 109.2 . . ?
B1 C9 H9B 109.2 . . ?
Si2 C5 Na1 115.60(9) . . ?
Si2 C5 H5 112.9(13) . . ?
Na1 C5 H5 73.0(14) . . ?
B1 C5 Si2 127.69(14) . . ?
B1 C5 Na1 95.47(11) . . ?
B1 C5 H5 116.1(13) . . ?
Si1 C4 H4A 108.4 . . ?
Si1 C4 H4B 108.4 . . ?
H4A C4 H4B 107.5 . . ?
B1 C4 Si1 115.48(13) . . ?
B1 C4 H4A 108.4 . . ?
B1 C4 H4B 108.4 . . ?
C9 B1 Na1 93.75(10) . . ?
C9 B1 C4 114.80(16) . . ?
C5 B1 Na1 55.82(9) . . ?
C5 B1 C9 121.82(16) . . ?
C5 B1 C4 123.37(16) . . ?
C4 B1 Na1 123.48(11) . . ?
Si2 C8 H8A 109.5 . . ?
Si2 C8 H8B 109.5 . . ?
Si2 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C13 H13A 109.5 . . ?
N1 C13 H13B 109.5 . . ?
N1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
Si3 C10 H10A 109.5 . . ?
Si3 C10 H10B 109.5 . . ?
Si3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si3 C12 H12A 109.5 . . ?
Si3 C12 H12B 109.5 . . ?
Si3 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N3 C19 H19A 108.7 . . ?
N3 C19 H19B 108.7 . . ?
H19A C19 H19B 107.6 . . ?
C18 C19 N3 114.4(2) . . ?
C18 C19 H19A 108.7 . . ?
C18 C19 H19B 108.7 . . ?
Si3 C11 H11A 109.5 . . ?
Si3 C11 H11B 109.5 . . ?
Si3 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C15 H15A 109 . . ?
N1 C15 H15B 109 . . ?
N1 C15 C16 113.0(2) . . ?
H15A C15 H15B 107.8 . . ?
C16 C15 H15A 109 . . ?
C16 C15 H15B 109 . . ?
Si1 C1 H1A 109.5 . . ?
Si1 C1 H1B 109.5 . . ?
Si1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N2 C16 H16A 108.8 . . ?
N2 C16 H16B 108.8 . . ?
C15 C16 N2 113.8(2) . . ?
C15 C16 H16A 108.8 . . ?
C15 C16 H16B 108.8 . . ?
H16A C16 H16B 107.7 . . ?
Si1 C3 H3A 109.5 . . ?
Si1 C3 H3B 109.5 . . ?
Si1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C2 H2A 109.5 . . ?
Si1 C2 H2B 109.5 . . ?
Si1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C17 H17A 109.5 . . ?
N2 C17 H17B 109.5 . . ?
N2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 113.2(2) . . ?
N2 C18 H18A 108.9 . . ?
N2 C18 H18B 108.9 . . ?
C19 C18 H18A 108.9 . . ?
C19 C18 H18B 108.9 . . ?
H18A C18 H18B 107.7 . . ?
N3 C21 H21A 109.5 . . ?
N3 C21 H21B 109.5 . . ?
N3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si2 C6 H6A 109.5 . . ?
Si2 C6 H6B 109.5 . . ?
Si2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
N1 C14 H14A 109.5 . . ?
N1 C14 H14B 109.5 . . ?
N1 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C7 H7A 109.5 . . ?
Si2 C7 H7B 109.5 . . ?
Si2 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C20 H20A 109.5 . . ?
N3 C20 H20B 109.5 . . ?
N3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si3 C9 B1 Na1 -137.40(9) . . . . ?
Si3 C9 B1 C5 -85.86(18) . . . . ?
Si3 C9 B1 C4 92.87(16) . . . . ?
Si1 C4 B1 Na1 -46.72(19) . . . . ?
Si1 C4 B1 C9 66.35(18) . . . . ?
Si1 C4 B1 C5 -114.94(18) . . . . ?
Si2 C5 B1 Na1 -128.49(18) . . . . ?
Si2 C5 B1 C9 160.68(14) . . . . ?
Si2 C5 B1 C4 -17.9(3) . . . . ?
Na1 N1 C15 C16 -45.3(3) . . . . ?
Na1 N3 C19 C18 -46.1(2) . . . . ?
Na1 N2 C16 C15 -42.0(3) . . . . ?
Na1 N2 C18 C19 -41.1(3) . . . . ?
Na1 C5 B1 C9 -70.83(16) . . . . ?
Na1 C5 B1 C4 110.55(16) . . . . ?
N1 C15 C16 N2 63.6(3) . . . . ?
N3 C19 C18 N2 63.6(3) . . . . ?
C8 Si2 C5 Na1 -174.96(11) . . . . ?
C8 Si2 C5 B1 -54.7(2) . . . . ?
C13 N1 C15 C16 78.7(3) . . . . ?
C10 Si3 C9 B1 73.66(16) . . . . ?
C12 Si3 C9 B1 -47.19(18) . . . . ?
C11 Si3 C9 B1 -167.18(15) . . . . ?
C1 Si1 C4 B1 -100.75(17) . . . . ?
C16 N2 C18 C19 -157.0(2) . . . . ?
C3 Si1 C4 B1 19.5(2) . . . . ?
C2 Si1 C4 B1 138.51(17) . . . . ?
C17 N2 C16 C15 -163.3(2) . . . . ?
C17 N2 C18 C19 81.8(3) . . . . ?
C18 N2 C16 C15 75.1(3) . . . . ?
C21 N3 C19 C18 -167.4(2) . . . . ?
C6 Si2 C5 Na1 -54.39(16) . . . . ?
C6 Si2 C5 B1 65.9(2) . . . . ?
C14 N1 C15 C16 -162.6(2) . . . . ?
C7 Si2 C5 Na1 66.50(15) . . . . ?
C7 Si2 C5 B1 -173.26(19) . . . . ?
C20 N3 C19 C18 71.2(3) . . . . ?


#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL AND FAB FILE                                   #
#----------------------------------------------------------------------------#


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_20EH146_MWS155
_database_code_depnum_ccdc_archive 'CCDC 2245608'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_audit_creation_date             2020-07-29
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C29 H55 B N3 Na Si2'
_chemical_formula_sum            'C29 H55 B N3 Na Si2'
_chemical_formula_weight         535.74
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C120 H212 B4 N8 Na4 Si8 '
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   11.08170(10)
_cell_length_b                   18.6842(2)
_cell_length_c                   16.2208(2)
_cell_angle_alpha                90
_cell_angle_beta                 93.3580(10)
_cell_angle_gamma                90
_cell_volume                     3352.79(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    15566
_cell_measurement_temperature    100.3(5)
_cell_measurement_theta_max      76.6680
_cell_measurement_theta_min      3.6010
_shelx_estimated_absorpt_T_max   0.936
_shelx_estimated_absorpt_T_min   0.828
_exptl_absorpt_coefficient_mu    1.227
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.65117
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.72a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1176
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.095
_exptl_crystal_size_min          0.055
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0411
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            32490
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.000
_diffrn_reflns_theta_min         3.612
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.3(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -34.00  52.00   1.00    0.50    --  -21.00  47.00 177.00   86
  2  ω    -93.00  -7.00   1.00    0.50    --  -21.00 -47.00  28.00   86
  3  ω    -23.00  50.00   1.00    0.50    --   47.89 -47.00  28.00   73
  4  ω     35.00 121.00   1.00    0.50    --   47.89  47.00 177.00   86
  5  ω     94.00 171.00   1.00    1.00    --  106.80  47.00 177.00   77
  6  ω    -92.00  -8.00   1.00    0.50    --  -21.00 -45.00 150.00   84
  7  ω    -68.00 -12.00   1.00    0.50    --  -21.00 125.00 -90.00   56
  8  ω    -26.00  23.00   1.00    0.50    --   47.89 -19.00-120.00   49
  9  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00  30.00   33
 10  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00 120.00   33
 11  ω     95.00 171.00   1.00    1.00    --  106.80  45.00  90.00   76
 12  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00  90.00   33
 13  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00-120.00   33
 14  ω     35.00 102.00   1.00    1.00    --  106.80 -77.00  90.00   67
 15  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00 150.00   33
 16  ω     35.00 102.00   1.00    1.00    --  106.80 -77.00   0.00   67
 17  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00 -60.00   33
 18  ω     35.00 106.00   1.00    1.00    --  106.80 -94.00-150.00   71
 19  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00   0.00   33
 20  ω     95.00 171.00   1.00    1.00    --  106.80  45.00 -90.00   76
 21  ω     95.00 171.00   1.00    1.00    --  106.80 125.00  30.00   76
 22  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00 -30.00   33
 23  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00 -90.00   33
 24  ω     35.00  68.00   1.00    1.00    --  106.80 -61.00-180.00   33
 25  ω     35.00 102.00   1.00    1.00    --  106.80 -77.00  30.00   67
 26  ω     26.00 121.00   1.00    0.50    --   47.89  77.00   0.00   95
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1379931000
_diffrn_orient_matrix_UB_12      0.0108112000
_diffrn_orient_matrix_UB_13      -0.0083883000
_diffrn_orient_matrix_UB_21      -0.0139240000
_diffrn_orient_matrix_UB_22      -0.0467182000
_diffrn_orient_matrix_UB_23      0.0771050000
_diffrn_orient_matrix_UB_31      0.0126283000
_diffrn_orient_matrix_UB_32      0.0670849000
_diffrn_orient_matrix_UB_33      0.0550715000
_diffrn_oxdiff_digest_frames     
;
01feacc35055c5b62f8c66d86d515f362a000371bc6
;
_diffrn_oxdiff_digest_hkl        
;
0106a8c953b5e480a0a300a22f85f604ea4486
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5830
_reflns_number_total             6931
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.72a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         6931
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0549
_refine_ls_restrained_S_all      1.071
_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)+(0.0806P)²+2.0287P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1574
_refine_special_details          ?
_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. Uiso/Uaniso restraints and constraints
Uanis(C26A) = Uanis(C26B) = Uanis(C27A) = Uanis(C27B)
3. Others
 Sof(C27B)=Sof(H27C)=Sof(H27D)=1-FVAR(1)
 Sof(C27A)=Sof(H27A)=Sof(H27B)=FVAR(1)
 Sof(C26B)=Sof(H26C)=Sof(H26D)=1-FVAR(2)
 Sof(C26A)=Sof(H26A)=Sof(H26B)=FVAR(2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C7(H7A,H7B), C23(H23A,H23B), C24(H24A,H24B), C26A(H26A,H26B),
 C27A(H27A,H27B), C27B(H27C,H27D), C26B(H26C,H26D)
4.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C15(H15), C16(H16), C19(H19), C5(H5), C4(H4), C3(H3),
 C17(H17), C18(H18)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C22(H22A,H22B,H22C), C12(H12A,H12B,H12C), C9(H9A,H9B,
 H9C), C29(H29A,H29B,H29C), C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C21(H21A,H21B,
 H21C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.28835(5) 0.55220(3) 0.59788(4) 0.03280(16) Uani 1 1 d . . . . .
Si2 Si 0.32466(5) 0.52742(3) 0.87158(4) 0.03432(16) Uani 1 1 d . . . . .
Na24 Na 0.73043(7) 0.72452(4) 0.75455(4) 0.02751(19) Uani 1 1 d . . . . .
N1 N 0.69742(17) 0.85293(9) 0.70804(11) 0.0354(4) Uani 1 1 d . . . . .
C1 C 0.55654(16) 0.62572(9) 0.68428(10) 0.0219(4) Uani 1 1 d . . . . .
C20 C 0.44573(16) 0.69420(10) 0.80031(12) 0.0248(4) Uani 1 1 d . . . . .
C11 C 0.44668(16) 0.54971(9) 0.80218(11) 0.0241(4) Uani 1 1 d . . . . .
H11A H 0.5224 0.5540 0.8374 0.029 Uiso 1 1 calc R . . . .
H11B H 0.4564 0.5077 0.7659 0.029 Uiso 1 1 calc R . . . .
C6 C 0.65701(17) 0.58046(10) 0.69267(12) 0.0276(4) Uani 1 1 d . . . . .
H6 H 0.6582 0.5442 0.7338 0.033 Uiso 1 1 calc R . . . .
N2 N 0.93690(18) 0.77448(13) 0.73636(14) 0.0496(5) Uani 1 1 d . . . . .
C2 C 0.56314(19) 0.67857(11) 0.62261(11) 0.0304(4) Uani 1 1 d . . . . .
H2 H 0.4982 0.7115 0.6148 0.037 Uiso 1 1 calc R . . . .
C15 C 0.53158(18) 0.70056(11) 0.86699(12) 0.0297(4) Uani 1 1 d . . . . .
H15 H 0.5877 0.6627 0.8769 0.036 Uiso 1 1 calc R . . . .
N3 N 0.87334(18) 0.67322(14) 0.87284(13) 0.0521(6) Uani 1 1 d . . . . .
C7 C 0.31355(17) 0.62141(10) 0.68022(13) 0.0298(4) Uani 1 1 d . . . . .
H7A H 0.3085 0.6687 0.6527 0.036 Uiso 1 1 calc R . . . .
H7B H 0.2445 0.6185 0.7161 0.036 Uiso 1 1 calc R . . . .
C16 C 0.5387(2) 0.75986(12) 0.91962(13) 0.0376(5) Uani 1 1 d . . . . .
H16 H 0.5985 0.7617 0.9640 0.045 Uiso 1 1 calc R . . . .
C19 C 0.36777(18) 0.75281(11) 0.78911(14) 0.0338(5) Uani 1 1 d . . . . .
H19 H 0.3089 0.7521 0.7441 0.041 Uiso 1 1 calc R . . . .
C5 C 0.7556(2) 0.58612(12) 0.64329(15) 0.0386(5) Uani 1 1 d . . . . .
H5 H 0.8218 0.5541 0.6511 0.046 Uiso 1 1 calc R . . . .
C4 C 0.7568(2) 0.63834(13) 0.58306(14) 0.0405(5) Uani 1 1 d . . . . .
H4 H 0.8234 0.6423 0.5491 0.049 Uiso 1 1 calc R . . . .
C3 C 0.6602(2) 0.68463(12) 0.57278(12) 0.0381(5) Uani 1 1 d . . . . .
H3 H 0.6602 0.7207 0.5315 0.046 Uiso 1 1 calc R . . . .
C10 C 0.3675(2) 0.46461(11) 0.61729(14) 0.0384(5) Uani 1 1 d . . . . .
H10A H 0.4550 0.4725 0.6224 0.058 Uiso 1 1 calc GR . . . .
H10B H 0.3478 0.4320 0.5711 0.058 Uiso 1 1 calc GR . . . .
H10C H 0.3410 0.4435 0.6685 0.058 Uiso 1 1 calc GR . . . .
C23 C 0.8139(2) 0.87414(12) 0.67619(13) 0.0378(5) Uani 1 1 d . . . . .
H23A H 0.8147 0.9268 0.6691 0.045 Uiso 1 1 calc R . . . .
H23B H 0.8208 0.8523 0.6211 0.045 Uiso 1 1 calc R . . . .
C17 C 0.4582(2) 0.81570(12) 0.90661(15) 0.0412(5) Uani 1 1 d . . . . .
H17 H 0.4616 0.8560 0.9423 0.049 Uiso 1 1 calc R . . . .
C18 C 0.3732(2) 0.81251(12) 0.84172(17) 0.0436(6) Uani 1 1 d . . . . .
H18 H 0.3178 0.8509 0.8324 0.052 Uiso 1 1 calc R . . . .
C22 C 0.6010(2) 0.86475(13) 0.64422(16) 0.0438(5) Uani 1 1 d . . . . .
H22A H 0.6168 0.8362 0.5953 0.066 Uiso 1 1 calc GR . . . .
H22B H 0.5980 0.9156 0.6294 0.066 Uiso 1 1 calc GR . . . .
H22C H 0.5234 0.8504 0.6651 0.066 Uiso 1 1 calc GR . . . .
C24 C 0.9214(2) 0.85262(14) 0.73082(15) 0.0466(6) Uani 1 1 d . . . . .
H24A H 0.9950 0.8740 0.7092 0.056 Uiso 1 1 calc R . . . .
H24B H 0.9124 0.8721 0.7869 0.056 Uiso 1 1 calc R . . . .
B1 B 0.43854(17) 0.62136(10) 0.74161(12) 0.0216(4) Uani 1 1 d . . . . .
C12 C 0.2892(2) 0.60369(14) 0.94075(15) 0.0441(5) Uani 1 1 d . . . . .
H12A H 0.3624 0.6177 0.9736 0.066 Uiso 1 1 calc GR . . . .
H12B H 0.2268 0.5889 0.9777 0.066 Uiso 1 1 calc GR . . . .
H12C H 0.2597 0.6444 0.9072 0.066 Uiso 1 1 calc GR . . . .
C9 C 0.3384(3) 0.58620(14) 0.49688(15) 0.0542(7) Uani 1 1 d . . . . .
H9A H 0.2934 0.6298 0.4815 0.081 Uiso 1 1 calc GR . . . .
H9B H 0.3228 0.5497 0.4542 0.081 Uiso 1 1 calc GR . . . .
H9C H 0.4250 0.5969 0.5021 0.081 Uiso 1 1 calc GR . . . .
C29 C 0.8472(3) 0.69594(14) 0.95544(17) 0.0570(7) Uani 1 1 d . . . . .
H29A H 0.8451 0.7483 0.9577 0.086 Uiso 1 1 calc GR . . . .
H29B H 0.9102 0.6781 0.9951 0.086 Uiso 1 1 calc GR . . . .
H29C H 0.7686 0.6768 0.9693 0.086 Uiso 1 1 calc GR . . . .
C8 C 0.1223(2) 0.53187(15) 0.5811(2) 0.0557(7) Uani 1 1 d . . . . .
H8A H 0.0930 0.5098 0.6309 0.084 Uiso 1 1 calc GR . . . .
H8B H 0.1096 0.4989 0.5344 0.084 Uiso 1 1 calc GR . . . .
H8C H 0.0778 0.5764 0.5691 0.084 Uiso 1 1 calc GR . . . .
C14 C 0.1784(2) 0.49833(17) 0.81785(19) 0.0576(8) Uani 1 1 d . . . . .
H14A H 0.1438 0.5381 0.7850 0.086 Uiso 1 1 calc GR . . . .
H14B H 0.1218 0.4839 0.8590 0.086 Uiso 1 1 calc GR . . . .
H14C H 0.1932 0.4578 0.7815 0.086 Uiso 1 1 calc GR . . . .
C21 C 0.6697(3) 0.89682(17) 0.77904(17) 0.0586(7) Uani 1 1 d . . . . .
H21A H 0.5892 0.8844 0.7967 0.088 Uiso 1 1 calc GR . . . .
H21B H 0.6712 0.9475 0.7636 0.088 Uiso 1 1 calc GR . . . .
H21C H 0.7301 0.8880 0.8245 0.088 Uiso 1 1 calc GR . . . .
C25 C 0.9925(2) 0.74833(16) 0.6621(2) 0.0622(8) Uani 1 1 d . . . . .
H25A H 0.9987 0.6960 0.6643 0.093 Uiso 1 1 calc GR . . . .
H25B H 1.0734 0.7691 0.6594 0.093 Uiso 1 1 calc GR . . . .
H25C H 0.9424 0.7624 0.6130 0.093 Uiso 1 1 calc GR . . . .
C28 C 0.8704(3) 0.59460(18) 0.87168(18) 0.0646(8) Uani 1 1 d . . . . .
H28A H 0.7894 0.5780 0.8837 0.097 Uiso 1 1 calc GR . . . .
H28B H 0.9296 0.5760 0.9135 0.097 Uiso 1 1 calc GR . . . .
H28C H 0.8903 0.5774 0.8170 0.097 Uiso 1 1 calc GR . . . .
C13 C 0.3714(3) 0.44882(16) 0.9390(2) 0.0679(9) Uani 1 1 d . . . . .
H13A H 0.3613 0.4045 0.9071 0.102 Uiso 1 1 calc GR . . . .
H13B H 0.3208 0.4470 0.9866 0.102 Uiso 1 1 calc GR . . . .
H13C H 0.4563 0.4541 0.9584 0.102 Uiso 1 1 calc GR . . . .
C26A C 1.0058(3) 0.7643(2) 0.8178(3) 0.0446(6) Uani 0.686(6) 1 d . . P A 2
H26A H 1.0830 0.7419 0.8040 0.054 Uiso 0.686(6) 1 calc R . P A 2
H26B H 1.0267 0.8134 0.8369 0.054 Uiso 0.686(6) 1 calc R . P A 2
C27A C 0.9963(3) 0.6868(2) 0.8437(3) 0.0446(6) Uani 0.660(5) 1 d . . P A 1
H27A H 1.0485 0.6944 0.8945 0.054 Uiso 0.660(5) 1 calc R . P A 1
H27B H 1.0220 0.6405 0.8206 0.054 Uiso 0.660(5) 1 calc R . P A 1
C27B C 0.9775(6) 0.7341(4) 0.8774(5) 0.0446(6) Uani 0.340(5) 1 d . . P A 2
H27C H 0.9522 0.7710 0.9167 0.054 Uiso 0.340(5) 1 calc R . P A 2
H27D H 1.0515 0.7115 0.9028 0.054 Uiso 0.340(5) 1 calc R . P A 2
C26B C 1.0291(7) 0.7333(5) 0.7938(6) 0.0446(6) Uani 0.314(6) 1 d . . P A 1
H26C H 1.0863 0.7096 0.7578 0.054 Uiso 0.314(6) 1 calc R . P A 1
H26D H 1.0761 0.7695 0.8266 0.054 Uiso 0.314(6) 1 calc R . P A 1


_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
Si1 C7 1.868(2) . ?
Si1 C10 1.875(2) . ?
Si1 C9 1.871(3) . ?
Si1 C8 1.883(3) . ?
Si2 C11 1.8567(19) . ?
Si2 C12 1.870(2) . ?
Si2 C14 1.875(3) . ?
Si2 C13 1.886(3) . ?
Na24 N1 2.535(2) . ?
Na24 C1 2.8570(18) . ?
Na24 C6 2.970(2) . ?
Na24 N2 2.504(2) . ?
Na24 C2 2.879(2) . ?
Na24 C15 2.976(2) . ?
Na24 N3 2.598(2) . ?
Na24 C3 3.096(2) . ?
N1 C23 1.472(3) . ?
N1 C22 1.460(3) . ?
N1 C21 1.461(3) . ?
C1 C6 1.398(3) . ?
C1 C2 1.411(3) . ?
C1 B1 1.650(3) . ?
C20 C15 1.403(3) . ?
C20 C19 1.400(3) . ?
C20 B1 1.660(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 B1 1.660(3) . ?
C6 H6 0.9500 . ?
C6 C5 1.396(3) . ?
N2 C24 1.472(4) . ?
N2 C25 1.468(4) . ?
N2 C26A 1.499(4) . ?
N2 C26B 1.547(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.388(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.398(3) . ?
N3 C29 1.451(4) . ?
N3 C28 1.469(4) . ?
N3 C27A 1.490(4) . ?
N3 C27B 1.618(7) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C7 B1 1.658(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.381(3) . ?
C19 H19 0.9500 . ?
C19 C18 1.404(3) . ?
C5 H5 0.9500 . ?
C5 C4 1.381(3) . ?
C4 H4 0.9500 . ?
C4 C3 1.378(4) . ?
C3 H3 0.9500 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.498(4) . ?
C17 H17 0.9500 . ?
C17 C18 1.372(4) . ?
C18 H18 0.9500 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C26A H26A 0.9900 . ?
C26A H26B 0.9900 . ?
C26A C27B 1.179(8) . ?
C27A H27A 0.9900 . ?
C27A H27B 0.9900 . ?
C27A C26B 1.255(10) . ?
C27B H27C 0.9900 . ?
C27B H27D 0.9900 . ?
C26B H26C 0.9900 . ?
C26B H26D 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C7 Si1 C10 115.81(9) . . ?
C7 Si1 C9 110.57(10) . . ?
C7 Si1 C8 110.31(12) . . ?
C10 Si1 C8 106.96(12) . . ?
C9 Si1 C10 106.49(13) . . ?
C9 Si1 C8 106.18(14) . . ?
C11 Si2 C12 112.28(9) . . ?
C11 Si2 C14 115.06(11) . . ?
C11 Si2 C13 109.97(12) . . ?
C12 Si2 C14 107.06(12) . . ?
C12 Si2 C13 107.79(14) . . ?
C14 Si2 C13 104.14(16) . . ?
N1 Na24 C1 114.24(6) . . ?
N1 Na24 C6 136.49(6) . . ?
N1 Na24 C2 89.17(6) . . ?
N1 Na24 C15 103.04(6) . . ?
N1 Na24 N3 129.79(8) . . ?
N1 Na24 C3 85.45(6) . . ?
C1 Na24 C6 27.69(5) . . ?
C1 Na24 C2 28.47(5) . . ?
C1 Na24 C15 68.96(5) . . ?
C1 Na24 C3 48.59(5) . . ?
C6 Na24 C15 82.69(5) . . ?
C6 Na24 C3 53.94(6) . . ?
N2 Na24 N1 74.28(7) . . ?
N2 Na24 C1 142.49(7) . . ?
N2 Na24 C6 122.15(7) . . ?
N2 Na24 C2 125.20(7) . . ?
N2 Na24 C15 147.43(7) . . ?
N2 Na24 N3 72.72(7) . . ?
N2 Na24 C3 99.08(7) . . ?
C2 Na24 C6 47.68(6) . . ?
C2 Na24 C15 86.73(6) . . ?
C2 Na24 C3 26.54(6) . . ?
C15 Na24 C3 113.19(6) . . ?
N3 Na24 C1 115.08(7) . . ?
N3 Na24 C6 93.34(7) . . ?
N3 Na24 C2 140.98(8) . . ?
N3 Na24 C15 86.16(7) . . ?
N3 Na24 C3 136.27(8) . . ?
C23 N1 Na24 104.18(13) . . ?
C22 N1 Na24 116.16(13) . . ?
C22 N1 C23 109.31(17) . . ?
C22 N1 C21 107.2(2) . . ?
C21 N1 Na24 109.26(16) . . ?
C21 N1 C23 110.77(18) . . ?
C6 C1 Na24 80.64(11) . . ?
C6 C1 C2 114.73(17) . . ?
C6 C1 B1 124.61(16) . . ?
C2 C1 Na24 76.64(10) . . ?
C2 C1 B1 120.65(16) . . ?
B1 C1 Na24 110.20(10) . . ?
C15 C20 B1 121.28(16) . . ?
C19 C20 C15 114.78(18) . . ?
C19 C20 B1 123.93(17) . . ?
Si2 C11 H11A 106.9 . . ?
Si2 C11 H11B 106.9 . . ?
H11A C11 H11B 106.7 . . ?
B1 C11 Si2 121.57(12) . . ?
B1 C11 H11A 106.9 . . ?
B1 C11 H11B 106.9 . . ?
Na24 C6 H6 114.6 . . ?
C1 C6 Na24 71.67(10) . . ?
C1 C6 H6 118.5 . . ?
C5 C6 Na24 85.26(12) . . ?
C5 C6 C1 122.94(19) . . ?
C5 C6 H6 118.5 . . ?
C24 N2 Na24 105.82(15) . . ?
C24 N2 C26A 103.3(2) . . ?
C24 N2 C26B 126.9(4) . . ?
C25 N2 Na24 113.74(16) . . ?
C25 N2 C24 109.4(2) . . ?
C25 N2 C26A 117.7(3) . . ?
C25 N2 C26B 92.0(5) . . ?
C26A N2 Na24 105.71(18) . . ?
C26B N2 Na24 108.6(3) . . ?
Na24 C2 H2 110.8 . . ?
C1 C2 Na24 74.89(10) . . ?
C1 C2 H2 118.5 . . ?
C3 C2 Na24 85.48(12) . . ?
C3 C2 C1 123.0(2) . . ?
C3 C2 H2 118.5 . . ?
Na24 C15 H15 73.4 . . ?
C20 C15 Na24 91.91(11) . . ?
C20 C15 H15 118.3 . . ?
C16 C15 Na24 103.76(13) . . ?
C16 C15 C20 123.3(2) . . ?
C16 C15 H15 118.3 . . ?
C29 N3 Na24 115.35(16) . . ?
C29 N3 C28 107.4(2) . . ?
C29 N3 C27A 118.6(3) . . ?
C29 N3 C27B 86.1(4) . . ?
C28 N3 Na24 110.33(16) . . ?
C28 N3 C27A 100.7(3) . . ?
C28 N3 C27B 135.9(3) . . ?
C27A N3 Na24 103.41(17) . . ?
C27B N3 Na24 100.2(3) . . ?
Si1 C7 H7A 107.1 . . ?
Si1 C7 H7B 107.1 . . ?
H7A C7 H7B 106.8 . . ?
B1 C7 Si1 120.90(13) . . ?
B1 C7 H7A 107.1 . . ?
B1 C7 H7B 107.1 . . ?
C15 C16 H16 120.2 . . ?
C17 C16 C15 119.5(2) . . ?
C17 C16 H16 120.2 . . ?
C20 C19 H19 118.7 . . ?
C20 C19 C18 122.6(2) . . ?
C18 C19 H19 118.7 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 C6 120.0(2) . . ?
C4 C5 H5 120.0 . . ?
C5 C4 H4 120.4 . . ?
C3 C4 C5 119.30(19) . . ?
C3 C4 H4 120.4 . . ?
Na24 C3 H3 119.3 . . ?
C2 C3 Na24 67.98(11) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 Na24 83.45(13) . . ?
C4 C3 C2 120.1(2) . . ?
C4 C3 H3 120.0 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N1 C23 H23A 108.8 . . ?
N1 C23 H23B 108.8 . . ?
N1 C23 C24 113.79(18) . . ?
H23A C23 H23B 107.7 . . ?
C24 C23 H23A 108.8 . . ?
C24 C23 H23B 108.8 . . ?
C16 C17 H17 120.2 . . ?
C18 C17 C16 119.52(19) . . ?
C18 C17 H17 120.2 . . ?
C19 C18 H18 119.9 . . ?
C17 C18 C19 120.3(2) . . ?
C17 C18 H18 119.9 . . ?
N1 C22 H22A 109.5 . . ?
N1 C22 H22B 109.5 . . ?
N1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N2 C24 C23 112.85(18) . . ?
N2 C24 H24A 109.0 . . ?
N2 C24 H24B 109.0 . . ?
C23 C24 H24A 109.0 . . ?
C23 C24 H24B 109.0 . . ?
H24A C24 H24B 107.8 . . ?
C1 B1 C20 105.64(13) . . ?
C1 B1 C11 110.85(14) . . ?
C1 B1 C7 108.86(15) . . ?
C11 B1 C20 108.82(14) . . ?
C7 B1 C20 110.75(14) . . ?
C7 B1 C11 111.75(15) . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N3 C29 H29A 109.5 . . ?
N3 C29 H29B 109.5 . . ?
N3 C29 H29C 109.5 . . ?
H29A C29 H29B 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si2 C14 H14A 109.5 . . ?
Si2 C14 H14B 109.5 . . ?
Si2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N1 C21 H21A 109.5 . . ?
N1 C21 H21B 109.5 . . ?
N1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C25 H25A 109.5 . . ?
N2 C25 H25B 109.5 . . ?
N2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N3 C28 H28A 109.5 . . ?
N3 C28 H28B 109.5 . . ?
N3 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N2 C26A H26A 104.9 . . ?
N2 C26A H26B 104.9 . . ?
H26A C26A H26B 105.8 . . ?
C27B C26A N2 129.6(4) . . ?
C27B C26A H26A 104.9 . . ?
C27B C26A H26B 104.9 . . ?
N3 C27A H27A 105.1 . . ?
N3 C27A H27B 105.1 . . ?
H27A C27A H27B 105.9 . . ?
C26B C27A N3 128.8(5) . . ?
C26B C27A H27A 105.1 . . ?
C26B C27A H27B 105.1 . . ?
N3 C27B H27C 106.9 . . ?
N3 C27B H27D 106.9 . . ?
C26A C27B N3 121.5(6) . . ?
C26A C27B H27C 106.9 . . ?
C26A C27B H27D 106.9 . . ?
H27C C27B H27D 106.7 . . ?
N2 C26B H26C 106.9 . . ?
N2 C26B H26D 106.9 . . ?
C27A C26B N2 121.8(6) . . ?
C27A C26B H26C 106.9 . . ?
C27A C26B H26D 106.9 . . ?
H26C C26B H26D 106.7 . . ?

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
Si1 C7 B1 C1 56.82(19) . . . . ?
Si1 C7 B1 C20 172.55(13) . . . . ?
Si1 C7 B1 C11 -66.0(2) . . . . ?
Si2 C11 B1 C1 -177.66(12) . . . . ?
Si2 C11 B1 C20 66.59(18) . . . . ?
Si2 C11 B1 C7 -56.0(2) . . . . ?
Na24 N1 C23 C24 -45.2(2) . . . . ?
Na24 C1 C6 C5 -71.43(18) . . . . ?
Na24 C1 C2 C3 74.18(18) . . . . ?
Na24 C1 B1 C20 17.86(15) . . . . ?
Na24 C1 B1 C11 -99.85(13) . . . . ?
Na24 C1 B1 C7 136.84(12) . . . . ?
Na24 C6 C5 C4 -64.4(2) . . . . ?
Na24 N2 C24 C23 -44.1(2) . . . . ?
Na24 N2 C26A C27B 6.3(8) . . . . ?
Na24 N2 C26B C27A -4.6(11) . . . . ?
Na24 C2 C3 C4 67.89(19) . . . . ?
Na24 C15 C16 C17 101.6(2) . . . . ?
Na24 N3 C27A C26B 24.5(8) . . . . ?
Na24 N3 C27B C26A -34.0(7) . . . . ?
N1 C23 C24 N2 66.0(3) . . . . ?
C1 C6 C5 C4 0.2(3) . . . . ?
C1 C2 C3 Na24 -68.72(16) . . . . ?
C1 C2 C3 C4 -0.8(3) . . . . ?
C20 C15 C16 C17 0.0(3) . . . . ?
C20 C19 C18 C17 0.9(3) . . . . ?
C6 C1 C2 Na24 -72.94(14) . . . . ?
C6 C1 C2 C3 1.2(3) . . . . ?
C6 C1 B1 C20 110.35(19) . . . . ?
C6 C1 B1 C11 -7.4(2) . . . . ?
C6 C1 B1 C7 -130.67(17) . . . . ?
C6 C5 C4 C3 0.3(3) . . . . ?
N2 C26A C27B N3 21.7(11) . . . . ?
C2 C1 C6 Na24 70.50(14) . . . . ?
C2 C1 C6 C5 -0.9(3) . . . . ?
C2 C1 B1 C20 -68.2(2) . . . . ?
C2 C1 B1 C11 174.06(15) . . . . ?
C2 C1 B1 C7 50.7(2) . . . . ?
C15 C20 C19 C18 -1.5(3) . . . . ?
C15 C20 B1 C1 -73.5(2) . . . . ?
C15 C20 B1 C11 45.6(2) . . . . ?
C15 C20 B1 C7 168.78(17) . . . . ?
C15 C16 C17 C18 -0.7(3) . . . . ?
N3 C27A C26B N2 -15.4(13) . . . . ?
C16 C17 C18 C19 0.2(3) . . . . ?
C19 C20 C15 Na24 -106.81(16) . . . . ?
C19 C20 C15 C16 1.0(3) . . . . ?
C19 C20 B1 C1 107.56(19) . . . . ?
C19 C20 B1 C11 -133.36(18) . . . . ?
C19 C20 B1 C7 -10.2(2) . . . . ?
C5 C4 C3 Na24 59.83(19) . . . . ?
C5 C4 C3 C2 0.0(3) . . . . ?
C10 Si1 C7 B1 26.5(2) . . . . ?
C22 N1 C23 C24 -170.0(2) . . . . ?
C24 N2 C26A C27B 117.3(7) . . . . ?
C24 N2 C26B C27A 123.2(8) . . . . ?
B1 C1 C6 Na24 -108.15(16) . . . . ?
B1 C1 C6 C5 -179.58(18) . . . . ?
B1 C1 C2 Na24 105.77(14) . . . . ?
B1 C1 C2 C3 179.96(17) . . . . ?
B1 C20 C15 Na24 74.16(16) . . . . ?
B1 C20 C15 C16 -177.98(18) . . . . ?
B1 C20 C19 C18 177.52(19) . . . . ?
C12 Si2 C11 B1 -53.95(18) . . . . ?
C9 Si1 C7 B1 -94.70(18) . . . . ?
C29 N3 C27A C26B -104.7(8) . . . . ?
C29 N3 C27B C26A -149.1(7) . . . . ?
C8 Si1 C7 B1 148.16(17) . . . . ?
C14 Si2 C11 B1 68.84(19) . . . . ?
C21 N1 C23 C24 72.2(3) . . . . ?
C25 N2 C24 C23 78.9(2) . . . . ?
C25 N2 C26A C27B -122.0(7) . . . . ?
C25 N2 C26B C27A -120.5(9) . . . . ?
C28 N3 C27A C26B 138.6(7) . . . . ?
C28 N3 C27B C26A 99.8(7) . . . . ?
C13 Si2 C11 B1 -173.97(18) . . . . ?
C26A N2 C24 C23 -155.0(2) . . . . ?
C26B N2 C24 C23 -173.0(5) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.818
_oxdiff_exptl_absorpt_empirical_full_min 0.673
####################################################################### 
# 
# 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_20EH113_MWS152
_database_code_depnum_ccdc_archive 'CCDC 2245610'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;

_audit_creation_date             2022-08-08T10:41:19-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C21 H55 B Li N3 Si3'
_chemical_formula_sum            'C21 H55 B Li N3 Si3'
_chemical_formula_weight         451.7
_chemical_absolute_configuration ad

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_Int_Tables_number      9
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   10.09239(18)
_cell_length_b                   17.0772(3)
_cell_length_c                   18.2578(3)
_cell_angle_alpha                90
_cell_angle_beta                 95.5490(17)
_cell_angle_gamma                90
_cell_volume                     3131.98(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    173.00(10)
_cell_measurement_reflns_used    24637
_cell_measurement_theta_min      4.866
_cell_measurement_theta_max      78.73

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       irregular
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_size_max          0.254
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.125
_exptl_crystal_density_diffrn    0.958
_exptl_crystal_F_000             1008

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.456
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.61a (Rigaku Oxford Diffraction, 2019)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.82982
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.709
_shelx_estimated_absorpt_T_max   0.839

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      173.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      -0.0302109
_diffrn_orient_matrix_ub_12      -0.0320639
_diffrn_orient_matrix_ub_13      -0.0787237
_diffrn_orient_matrix_ub_21      0.1320649
_diffrn_orient_matrix_ub_22      0.0345024
_diffrn_orient_matrix_ub_23      -0.0211878
_diffrn_orient_matrix_ub_31      0.0718525
_diffrn_orient_matrix_ub_32      -0.0769176
_diffrn_orient_matrix_ub_33      0.0233382
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_number            31296
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.867
_diffrn_reflns_theta_max         80.244
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.971
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.949
_reflns_Friedel_coverage         0.952
_reflns_number_total             6654
_reflns_number_gt                6333
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0875P)²+1.0043P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         6654
_refine_ls_number_parameters     329
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0501
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1436
_refine_ls_wR_factor_gt          0.1382
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_restrained_S_all      1.125
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_abs_structure_details 
;
 Flack x determined using 2919 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.03(3)
_refine_diff_density_max         0.299
_refine_diff_density_min         -0.157
_refine_diff_density_rms         0.041

#----------------------------------------------------------------------------#
#                   SQUEEZE                                                  #
#----------------------------------------------------------------------------#

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.014 0.141 0.336 14.1 0.0 ?
2 0.056 0.356 0.635 7.2 0.0 ?
3 0.056 0.644 0.135 7.2 0.0 ?
4 0.014 0.859 0.836 14.1 0.0 ?
5 0.148 0.000 0.146 7.2 0.0 ?
6 0.148 0.000 0.646 7.2 0.0 ?
7 0.514 0.359 0.836 14.1 0.0 ?
8 0.514 0.641 0.336 14.1 0.0 ?
9 0.556 0.144 0.135 7.2 0.0 ?
10 0.556 0.856 0.635 7.2 0.0 ?
11 0.648 0.500 0.146 7.2 0.0 ?
12 0.648 0.500 0.646 7.2 0.0 ?

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2


#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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 0.25488(13) 0.29110(5) 0.48614(8) 0.0472(2) Uani 1 1 d . . . . .
Si3 Si 0.65525(13) 0.42906(5) 0.39664(8) 0.0492(2) Uani 1 1 d . . . . .
Si2 Si 0.64359(14) 0.16345(6) 0.36801(8) 0.0494(2) Uani 1 1 d . . . . .
N3 N 0.6527(4) 0.28549(19) 0.62347(18) 0.0530(7) Uani 1 1 d . . . . .
N1 N 0.4981(3) 0.09325(19) 0.64549(16) 0.0575(7) Uani 1 1 d D U . . .
C18 C 0.5334(4) 0.3502(2) 0.4131(2) 0.0465(7) Uani 1 1 d . . . . .
H18A H 0.448015 0.376409 0.420062 0.056 Uiso 1 1 calc R U . . .
H18B H 0.518641 0.319701 0.3669 0.056 Uiso 1 1 calc R U . . .
N2 N 0.7766(4) 0.1287(2) 0.6412(2) 0.0551(7) Uani 1 1 d . . . . .
C14 C 0.6684(4) 0.2171(2) 0.4575(2) 0.0448(7) Uani 1 1 d . . . . .
H14A H 0.760767 0.238839 0.463845 0.054 Uiso 1 1 calc R U . . .
C10 C 0.4198(4) 0.2417(2) 0.5026(2) 0.0444(7) Uani 1 1 d . . . . .
C9 C 0.6205(4) 0.3344(2) 0.5556(2) 0.0486(7) Uani 1 1 d . . . . .
C5 C 0.8777(4) 0.0979(3) 0.5963(3) 0.0627(10) Uani 1 1 d . . . . .
H5A H 0.953821 0.078406 0.628551 0.094 Uiso 1 1 calc R U . . .
H5B H 0.907312 0.139754 0.564946 0.094 Uiso 1 1 calc R U . . .
H5C H 0.839532 0.05506 0.565414 0.094 Uiso 1 1 calc R U . . .
C7 C 0.7989(5) 0.2717(3) 0.6372(3) 0.0621(10) Uani 1 1 d . . . . .
C6 C 0.8267(6) 0.1984(3) 0.6825(3) 0.0681(11) Uani 1 1 d . . . . .
H6A H 0.923743 0.193137 0.695692 0.082 Uiso 1 1 calc R U . . .
H6B H 0.783086 0.202386 0.728697 0.082 Uiso 1 1 calc R U . . .
C21 C 0.8362(4) 0.3987(3) 0.4063(3) 0.0646(11) Uani 1 1 d . . . . .
H21A H 0.847379 0.352025 0.376331 0.097 Uiso 1 1 calc R U . . .
H21B H 0.864271 0.386939 0.458043 0.097 Uiso 1 1 calc R U . . .
H21C H 0.890723 0.441431 0.389648 0.097 Uiso 1 1 calc R U . . .
C13 C 0.2563(5) 0.3918(3) 0.5272(3) 0.0718(12) Uani 1 1 d . . . . .
H13A H 0.318257 0.425129 0.503121 0.108 Uiso 1 1 calc R U . . .
H13B H 0.284803 0.388726 0.579976 0.108 Uiso 1 1 calc R U . . .
H13C H 0.16664 0.414283 0.519949 0.108 Uiso 1 1 calc R U . . .
B1 B 0.5609(4) 0.2861(2) 0.4808(2) 0.0416(7) Uani 1 1 d . . . . .
C4 C 0.7328(5) 0.0670(3) 0.6897(3) 0.0711(12) Uani 1 1 d D . . . .
H4AA H 0.79478 0.06504 0.735111 0.085 Uiso 0.824(13) 1 calc R U P A 1
H4AB H 0.736918 0.015788 0.664621 0.085 Uiso 0.824(13) 1 calc R U P A 1
H4BC H 0.727368 0.089134 0.739425 0.085 Uiso 0.176(13) 1 calc R U P A 2
H4BD H 0.800161 0.024707 0.693918 0.085 Uiso 0.176(13) 1 calc R U P A 2
C20 C 0.6374(5) 0.5149(3) 0.4597(3) 0.0676(11) Uani 1 1 d . . . . .
H20A H 0.658364 0.498239 0.51087 0.101 Uiso 1 1 calc R U . . .
H20B H 0.545817 0.534466 0.452887 0.101 Uiso 1 1 calc R U . . .
H20C H 0.698858 0.556513 0.448106 0.101 Uiso 1 1 calc R U . . .
C12 C 0.1921(5) 0.2977(4) 0.3866(3) 0.0735(13) Uani 1 1 d . . . . .
H12A H 0.180647 0.244847 0.366075 0.11 Uiso 1 1 calc R U . . .
H12B H 0.256301 0.326615 0.360066 0.11 Uiso 1 1 calc R U . . .
H12C H 0.106342 0.325074 0.381612 0.11 Uiso 1 1 calc R U . . .
C19 C 0.6181(5) 0.4690(3) 0.3011(3) 0.0712(12) Uani 1 1 d . . . . .
H19A H 0.525484 0.487003 0.294354 0.107 Uiso 1 1 calc R U . . .
H19B H 0.631535 0.427829 0.265164 0.107 Uiso 1 1 calc R U . . .
H19C H 0.677739 0.513009 0.293882 0.107 Uiso 1 1 calc R U . . .
C11 C 0.1242(4) 0.2363(3) 0.5324(3) 0.0716(12) Uani 1 1 d . . . . .
H11A H 0.146528 0.23739 0.585826 0.107 Uiso 1 1 calc R U . . .
H11B H 0.120786 0.181852 0.515285 0.107 Uiso 1 1 calc R U . . .
H11C H 0.037299 0.261041 0.520138 0.107 Uiso 1 1 calc R U . . .
C17 C 0.7062(7) 0.2202(4) 0.2898(3) 0.0876(16) Uani 1 1 d . . . . .
H17A H 0.801122 0.231592 0.30126 0.131 Uiso 1 1 calc R U . . .
H17B H 0.656611 0.269378 0.282933 0.131 Uiso 1 1 calc R U . . .
H17C H 0.693493 0.189046 0.244588 0.131 Uiso 1 1 calc R U . . .
C16 C 0.4663(5) 0.1366(3) 0.3380(3) 0.0698(11) Uani 1 1 d . . . . .
H16A H 0.412284 0.184319 0.332176 0.105 Uiso 1 1 calc R U . . .
H16B H 0.431836 0.102858 0.375193 0.105 Uiso 1 1 calc R U . . .
H16C H 0.462143 0.1087 0.290936 0.105 Uiso 1 1 calc R U . . .
C8 C 0.6019(8) 0.3227(3) 0.6874(3) 0.0839(16) Uani 1 1 d . . . . .
H8A H 0.504528 0.32558 0.6798 0.126 Uiso 1 1 calc R U . . .
H8B H 0.638709 0.37561 0.693549 0.126 Uiso 1 1 calc R U . . .
H8C H 0.62833 0.291679 0.731561 0.126 Uiso 1 1 calc R U . . .
C3 C 0.5939(5) 0.0798(4) 0.7102(3) 0.0690(16) Uani 0.824(13) 1 d D U P A 1
H3A H 0.565684 0.03347 0.737252 0.083 Uiso 0.824(13) 1 calc R U P A 1
H3B H 0.593384 0.125627 0.743398 0.083 Uiso 0.824(13) 1 calc R U P A 1
C15 C 0.7401(7) 0.0693(4) 0.3756(4) 0.096(2) Uani 1 1 d . . . . .
H15A H 0.70428 0.03534 0.412241 0.144 Uiso 1 1 calc R U . . .
H15B H 0.833997 0.080498 0.390794 0.144 Uiso 1 1 calc R U . . .
H15C H 0.732468 0.042786 0.32776 0.144 Uiso 1 1 calc R U . . .
C1 C 0.4749(9) 0.0249(4) 0.5971(5) 0.082(2) Uani 0.824(13) 1 d D . P A 1
H1A H 0.410271 0.038477 0.555495 0.123 Uiso 0.824(13) 1 calc R U P A 1
H1B H 0.558913 0.008965 0.578704 0.123 Uiso 0.824(13) 1 calc R U P A 1
H1C H 0.440041 -0.018401 0.624794 0.123 Uiso 0.824(13) 1 calc R U P A 1
C2 C 0.3692(7) 0.1159(5) 0.6705(5) 0.089(3) Uani 0.824(13) 1 d D . P A 1
H2A H 0.381427 0.161481 0.703027 0.133 Uiso 0.824(13) 1 calc R U P A 1
H2B H 0.306724 0.128997 0.627826 0.133 Uiso 0.824(13) 1 calc R U P A 1
H2C H 0.33361 0.072152 0.69736 0.133 Uiso 0.824(13) 1 calc R U P A 1
Li1 Li 0.5951(7) 0.1788(4) 0.5873(4) 0.0498(13) Uani 1 1 d . . . . .
H9A H 0.555(4) 0.373(2) 0.567(2) 0.043(10) Uiso 1 1 d . . . . .
H9B H 0.705(5) 0.364(3) 0.547(3) 0.054(12) Uiso 1 1 d . . . . .
H7A H 0.848(5) 0.315(3) 0.662(3) 0.059(13) Uiso 1 1 d . . . . .
H7B H 0.830(5) 0.266(3) 0.586(3) 0.058(12) Uiso 1 1 d . . . . .
H10A H 0.403(5) 0.193(3) 0.484(3) 0.057(12) Uiso 1 1 d . . . . .
H10B H 0.424(5) 0.232(3) 0.557(3) 0.062(13) Uiso 1 1 d . . . . .
H14B H 0.675(5) 0.171(3) 0.494(3) 0.052(11) Uiso 1 1 d . . . . .
C2A C 0.431(4) 0.125(2) 0.7073(18) 0.090(11) Uani 0.176(13) 1 d D U P A 2
H2AA H 0.494165 0.156786 0.738577 0.135 Uiso 0.176(13) 1 calc R U P A 2
H2AB H 0.355158 0.156545 0.688324 0.135 Uiso 0.176(13) 1 calc R U P A 2
H2AC H 0.400463 0.081053 0.736305 0.135 Uiso 0.176(13) 1 calc R U P A 2
C1A C 0.413(3) 0.0437(17) 0.5947(15) 0.077(9) Uani 0.176(13) 1 d D U P A 2
H1AA H 0.463998 0.025117 0.555172 0.115 Uiso 0.176(13) 1 calc R U P A 2
H1AB H 0.381592 -0.001298 0.621597 0.115 Uiso 0.176(13) 1 calc R U P A 2
H1AC H 0.336286 0.074194 0.573616 0.115 Uiso 0.176(13) 1 calc R U P A 2
C3A C 0.6002(11) 0.0328(4) 0.6625(18) 0.085(10) Uani 0.176(13) 1 d D U P A 2
H3AA H 0.609846 0.001438 0.617725 0.102 Uiso 0.176(13) 1 calc R U P A 2
H3AB H 0.57063 -0.002877 0.700494 0.102 Uiso 0.176(13) 1 calc R U P A 2



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Si1 C10 1.864(4) . ?
Si1 C13 1.876(5) . ?
Si1 C12 1.869(5) . ?
Si1 C11 1.883(4) . ?
Si3 C18 1.868(4) . ?
Si3 C21 1.890(4) . ?
Si3 C20 1.882(5) . ?
Si3 C19 1.877(5) . ?
Si2 C14 1.869(4) . ?
Si2 C17 1.884(5) . ?
Si2 C16 1.877(5) . ?
Si2 C15 1.879(5) . ?
N3 C9 1.504(5) . ?
N3 C7 1.491(6) . ?
N3 C8 1.464(5) . ?
N3 Li1 2.005(7) . ?
N1 C3 1.469(4) . ?
N1 C1 1.469(4) . ?
N1 C2 1.472(4) . ?
N1 Li1 2.103(7) . ?
N1 C2A 1.470(4) . ?
N1 C1A 1.470(4) . ?
N1 C3A 1.470(4) . ?
C18 H18A 0.99 . ?
C18 H18B 0.99 . ?
C18 B1 1.654(5) . ?
N2 C5 1.466(6) . ?
N2 C6 1.472(6) . ?
N2 C4 1.471(6) . ?
N2 Li1 2.169(7) . ?
C14 H14A 1 . ?
C14 B1 1.683(5) . ?
C14 Li1 2.633(7) . ?
C14 H14B 1.03(5) . ?
C10 B1 1.694(5) . ?
C10 Li1 2.480(8) . ?
C10 H10A 0.90(5) . ?
C10 H10B 1.01(6) . ?
C9 B1 1.658(5) . ?
C9 Li1 2.737(7) . ?
C9 H9A 0.96(4) . ?
C9 H9B 1.02(5) . ?
C5 H5A 0.98 . ?
C5 H5B 0.98 . ?
C5 H5C 0.98 . ?
C7 C6 1.512(6) . ?
C7 Li1 2.685(8) . ?
C7 H7A 0.98(5) . ?
C7 H7B 1.01(5) . ?
C6 H6A 0.99 . ?
C6 H6B 0.99 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
B1 Li1 2.671(7) . ?
C4 H4AA 0.99 . ?
C4 H4AB 0.99 . ?
C4 H4BC 0.99 . ?
C4 H4BD 0.99 . ?
C4 C3 1.502(7) . ?
C4 C3A 1.500(8) . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C16 H16A 0.98 . ?
C16 H16B 0.98 . ?
C16 H16C 0.98 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C3 H3A 0.99 . ?
C3 H3B 0.99 . ?
C15 H15A 0.98 . ?
C15 H15B 0.98 . ?
C15 H15C 0.98 . ?
C1 H1A 0.98 . ?
C1 H1B 0.98 . ?
C1 H1C 0.98 . ?
C2 H2A 0.98 . ?
C2 H2B 0.98 . ?
C2 H2C 0.98 . ?
Li1 H10B 1.98(5) . ?
Li1 H14B 1.96(5) . ?
C2A H2AA 0.98 . ?
C2A H2AB 0.98 . ?
C2A H2AC 0.98 . ?
C1A H1AA 0.98 . ?
C1A H1AB 0.98 . ?
C1A H1AC 0.98 . ?
C3A H3AA 0.99 . ?
C3A H3AB 0.99 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C10 Si1 C13 112.2(2) . . ?
C10 Si1 C12 113.43(19) . . ?
C10 Si1 C11 110.85(19) . . ?
C13 Si1 C11 104.8(2) . . ?
C12 Si1 C13 108.8(3) . . ?
C12 Si1 C11 106.2(3) . . ?
C18 Si3 C21 115.62(18) . . ?
C18 Si3 C20 111.1(2) . . ?
C18 Si3 C19 109.6(2) . . ?
C20 Si3 C21 107.7(2) . . ?
C19 Si3 C21 106.9(2) . . ?
C19 Si3 C20 105.3(2) . . ?
C14 Si2 C17 112.6(2) . . ?
C14 Si2 C16 114.71(19) . . ?
C14 Si2 C15 109.3(2) . . ?
C16 Si2 C17 106.5(3) . . ?
C16 Si2 C15 106.6(3) . . ?
C15 Si2 C17 106.7(3) . . ?
C9 N3 Li1 101.6(3) . . ?
C7 N3 C9 111.0(3) . . ?
C7 N3 Li1 99.3(3) . . ?
C8 N3 C9 110.6(3) . . ?
C8 N3 C7 110.6(4) . . ?
C8 N3 Li1 122.9(4) . . ?
C3 N1 C2 108.9(5) . . ?
C3 N1 Li1 102.2(3) . . ?
C1 N1 C3 114.4(5) . . ?
C1 N1 C2 107.5(6) . . ?
C1 N1 Li1 107.6(4) . . ?
C2 N1 Li1 116.3(4) . . ?
C2A N1 Li1 114.0(16) . . ?
C2A N1 C1A 114(2) . . ?
C2A N1 C3A 117(2) . . ?
C1A N1 Li1 110.7(13) . . ?
C1A N1 C3A 94.8(16) . . ?
C3A N1 Li1 104.1(10) . . ?
Si3 C18 H18A 106.8 . . ?
Si3 C18 H18B 106.8 . . ?
H18A C18 H18B 106.6 . . ?
B1 C18 Si3 122.1(2) . . ?
B1 C18 H18A 106.8 . . ?
B1 C18 H18B 106.8 . . ?
C5 N2 C6 110.7(4) . . ?
C5 N2 C4 110.2(4) . . ?
C5 N2 Li1 119.3(3) . . ?
C6 N2 Li1 98.4(3) . . ?
C4 N2 C6 112.2(4) . . ?
C4 N2 Li1 105.4(3) . . ?
Si2 C14 H14A 109.1 . . ?
Si2 C14 Li1 129.8(2) . . ?
Si2 C14 H14B 101(3) . . ?
H14A C14 H14B 101.7 . . ?
B1 C14 Si2 121.9(2) . . ?
B1 C14 H14A 109.1 . . ?
B1 C14 Li1 72.7(2) . . ?
B1 C14 H14B 112(3) . . ?
Li1 C14 H14A 109.1 . . ?
Si1 C10 Li1 150.3(2) . . ?
Si1 C10 H10A 103(3) . . ?
Si1 C10 H10B 101(3) . . ?
B1 C10 Si1 121.1(2) . . ?
B1 C10 Li1 77.0(2) . . ?
B1 C10 H10A 117(3) . . ?
B1 C10 H10B 111(3) . . ?
Li1 C10 H10A 86(3) . . ?
Li1 C10 H10B 50(3) . . ?
H10A C10 H10B 102(4) . . ?
N3 C9 B1 115.8(3) . . ?
N3 C9 Li1 45.9(2) . . ?
N3 C9 H9A 107(3) . . ?
N3 C9 H9B 107(3) . . ?
B1 C9 Li1 70.0(2) . . ?
B1 C9 H9A 108(3) . . ?
B1 C9 H9B 111(3) . . ?
Li1 C9 H9A 122(3) . . ?
Li1 C9 H9B 128(3) . . ?
H9A C9 H9B 107(4) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N3 C7 C6 110.6(4) . . ?
N3 C7 Li1 47.5(2) . . ?
N3 C7 H7A 114(3) . . ?
N3 C7 H7B 105(3) . . ?
C6 C7 Li1 78.0(3) . . ?
C6 C7 H7A 109(3) . . ?
C6 C7 H7B 111(3) . . ?
Li1 C7 H7A 161(3) . . ?
Li1 C7 H7B 86(3) . . ?
H7A C7 H7B 107(4) . . ?
N2 C6 C7 110.6(3) . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
C7 C6 H6A 109.5 . . ?
C7 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si1 C13 H13A 109.5 . . ?
Si1 C13 H13B 109.5 . . ?
Si1 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C18 B1 C14 109.9(3) . . ?
C18 B1 C10 112.8(3) . . ?
C18 B1 C9 107.9(3) . . ?
C18 B1 Li1 177.3(3) . . ?
C14 B1 C10 108.9(3) . . ?
C14 B1 Li1 70.3(2) . . ?
C10 B1 Li1 64.8(2) . . ?
C9 B1 C14 111.4(3) . . ?
C9 B1 C10 105.9(3) . . ?
C9 B1 Li1 74.4(2) . . ?
N2 C4 H4AA 109 . . ?
N2 C4 H4AB 109 . . ?
N2 C4 H4BC 109 . . ?
N2 C4 H4BD 109 . . ?
N2 C4 C3 112.8(4) . . ?
N2 C4 C3A 113.0(11) . . ?
H4AA C4 H4AB 107.8 . . ?
H4BC C4 H4BD 107.8 . . ?
C3 C4 H4AA 109 . . ?
C3 C4 H4AB 109 . . ?
C3A C4 H4BC 109 . . ?
C3A C4 H4BD 109 . . ?
Si3 C20 H20A 109.5 . . ?
Si3 C20 H20B 109.5 . . ?
Si3 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C12 H12A 109.5 . . ?
Si1 C12 H12B 109.5 . . ?
Si1 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si3 C19 H19A 109.5 . . ?
Si3 C19 H19B 109.5 . . ?
Si3 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
Si1 C11 H11A 109.5 . . ?
Si1 C11 H11B 109.5 . . ?
Si1 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C17 H17A 109.5 . . ?
Si2 C17 H17B 109.5 . . ?
Si2 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C16 H16A 109.5 . . ?
Si2 C16 H16B 109.5 . . ?
Si2 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N3 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
N3 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C3 C4 112.3(4) . . ?
N1 C3 H3A 109.1 . . ?
N1 C3 H3B 109.1 . . ?
C4 C3 H3A 109.1 . . ?
C4 C3 H3B 109.1 . . ?
H3A C3 H3B 107.9 . . ?
Si2 C15 H15A 109.5 . . ?
Si2 C15 H15B 109.5 . . ?
Si2 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N3 Li1 N1 126.8(3) . . ?
N3 Li1 N2 90.2(3) . . ?
N3 Li1 C14 88.4(3) . . ?
N3 Li1 C10 88.7(3) . . ?
N3 Li1 C9 32.57(16) . . ?
N3 Li1 C7 33.22(18) . . ?
N3 Li1 B1 68.2(2) . . ?
N3 Li1 H10B 83.8(15) . . ?
N3 Li1 H14B 102.5(14) . . ?
N1 Li1 N2 84.9(3) . . ?
N1 Li1 C14 144.3(3) . . ?
N1 Li1 C10 106.1(3) . . ?
N1 Li1 C9 147.0(3) . . ?
N1 Li1 C7 128.1(3) . . ?
N1 Li1 B1 144.2(3) . . ?
N1 Li1 H10B 91.3(15) . . ?
N1 Li1 H14B 130.0(14) . . ?
N2 Li1 C14 102.0(3) . . ?
N2 Li1 C10 166.9(3) . . ?
N2 Li1 C9 112.7(3) . . ?
N2 Li1 C7 59.6(2) . . ?
N2 Li1 B1 130.2(3) . . ?
N2 Li1 H10B 169.0(17) . . ?
N2 Li1 H14B 87.9(14) . . ?
C14 Li1 C9 61.83(17) . . ?
C14 Li1 C7 83.5(2) . . ?
C14 Li1 B1 37.00(13) . . ?
C14 Li1 H10B 87.1(16) . . ?
C14 Li1 H14B 19.9(14) . . ?
C10 Li1 C14 64.93(19) . . ?
C10 Li1 C9 61.50(18) . . ?
C10 Li1 C7 115.6(3) . . ?
C10 Li1 B1 38.19(15) . . ?
C10 Li1 H10B 22.8(16) . . ?
C10 Li1 H14B 79.6(14) . . ?
C9 Li1 H10B 66.0(15) . . ?
C9 Li1 H14B 80.1(14) . . ?
C7 Li1 C9 54.14(18) . . ?
C7 Li1 H10B 116.2(15) . . ?
C7 Li1 H14B 88.1(14) . . ?
B1 Li1 C9 35.69(14) . . ?
B1 Li1 C7 83.3(2) . . ?
B1 Li1 H10B 55.6(16) . . ?
B1 Li1 H14B 56.6(14) . . ?
H10B Li1 H14B 102(2) . . ?
N1 C2A H2AA 109.5 . . ?
N1 C2A H2AB 109.5 . . ?
N1 C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
N1 C1A H1AA 109.5 . . ?
N1 C1A H1AB 109.5 . . ?
N1 C1A H1AC 109.5 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
N1 C3A C4 112.3(5) . . ?
N1 C3A H3AA 109.1 . . ?
N1 C3A H3AB 109.1 . . ?
C4 C3A H3AA 109.1 . . ?
C4 C3A H3AB 109.1 . . ?
H3AA C3A H3AB 107.9 . . ?

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
Si1 C10 B1 C18 -27.0(4) . . . . ?
Si1 C10 B1 C14 -149.2(2) . . . . ?
Si1 C10 B1 C9 90.9(3) . . . . ?
Si1 C10 B1 Li1 154.5(3) . . . . ?
Si3 C18 B1 C14 -77.9(4) . . . . ?
Si3 C18 B1 C10 160.5(2) . . . . ?
Si3 C18 B1 C9 43.8(4) . . . . ?
Si2 C14 B1 C18 -50.6(4) . . . . ?
Si2 C14 B1 C10 73.4(3) . . . . ?
Si2 C14 B1 C9 -170.1(2) . . . . ?
Si2 C14 B1 Li1 126.5(3) . . . . ?
N3 C9 B1 C18 -179.6(3) . . . . ?
N3 C9 B1 C14 -58.9(4) . . . . ?
N3 C9 B1 C10 59.3(4) . . . . ?
N3 C9 B1 Li1 2.0(3) . . . . ?
N3 C7 C6 N2 65.3(5) . . . . ?
N2 C4 C3 N1 51.6(7) . . . . ?
N2 C4 C3A N1 -51(2) . . . . ?
C9 N3 C7 C6 -156.1(3) . . . . ?
C9 N3 C7 Li1 -106.3(3) . . . . ?
C5 N2 C6 C7 87.9(5) . . . . ?
C5 N2 C4 C3 -153.5(5) . . . . ?
C5 N2 C4 C3A -102.5(10) . . . . ?
C7 N3 C9 B1 102.2(4) . . . . ?
C7 N3 C9 Li1 104.8(4) . . . . ?
C6 N2 C4 C3 82.6(5) . . . . ?
C6 N2 C4 C3A 133.6(10) . . . . ?
C21 Si3 C18 B1 41.4(4) . . . . ?
C13 Si1 C10 B1 -52.2(3) . . . . ?
C13 Si1 C10 Li1 69.9(5) . . . . ?
C4 N2 C6 C7 -148.4(4) . . . . ?
C20 Si3 C18 B1 -81.7(3) . . . . ?
C12 Si1 C10 B1 71.6(3) . . . . ?
C12 Si1 C10 Li1 -166.4(5) . . . . ?
C19 Si3 C18 B1 162.4(3) . . . . ?
C11 Si1 C10 B1 -169.0(3) . . . . ?
C11 Si1 C10 Li1 -46.9(5) . . . . ?
C17 Si2 C14 B1 82.7(4) . . . . ?
C17 Si2 C14 Li1 176.3(3) . . . . ?
C16 Si2 C14 B1 -39.4(3) . . . . ?
C16 Si2 C14 Li1 54.3(3) . . . . ?
C8 N3 C9 B1 -134.6(4) . . . . ?
C8 N3 C9 Li1 -132.1(5) . . . . ?
C8 N3 C7 C6 80.8(5) . . . . ?
C8 N3 C7 Li1 130.6(4) . . . . ?
C15 Si2 C14 B1 -159.0(4) . . . . ?
C15 Si2 C14 Li1 -65.4(4) . . . . ?
C1 N1 C3 C4 67.4(7) . . . . ?
C2 N1 C3 C4 -172.3(6) . . . . ?
Li1 N3 C9 B1 -2.6(4) . . . . ?
Li1 N3 C7 C6 -49.8(4) . . . . ?
Li1 N1 C3 C4 -48.7(5) . . . . ?
Li1 N1 C3A C4 44(2) . . . . ?
Li1 N2 C6 C7 -37.9(5) . . . . ?
Li1 N2 C4 C3 -23.5(6) . . . . ?
Li1 N2 C4 C3A 27.5(10) . . . . ?
Li1 C14 B1 C18 -177.1(3) . . . . ?
Li1 C14 B1 C10 -53.1(3) . . . . ?
Li1 C14 B1 C9 63.4(3) . . . . ?
Li1 C10 B1 C18 178.6(3) . . . . ?
Li1 C10 B1 C14 56.3(3) . . . . ?
Li1 C10 B1 C9 -63.6(3) . . . . ?
Li1 C9 B1 C18 178.4(3) . . . . ?
Li1 C9 B1 C14 -60.9(3) . . . . ?
Li1 C9 B1 C10 57.3(2) . . . . ?
Li1 C7 C6 N2 30.1(4) . . . . ?
C2A N1 C3A C4 -82(3) . . . . ?
C1A N1 C3A C4 157(2) . . . . ?


#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL AND FAB FILE                                   #
#----------------------------------------------------------------------------#


# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_20EH127_MWS141_2
_database_code_depnum_ccdc_archive 'CCDC 2245607'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;

_audit_creation_date             2023-02-23T17:34:48-00:00

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_formula_moiety         'C27 H61 B N3 Na Si3'
_chemical_formula_sum            'C27 H61 B N3 Na Si3'
_chemical_formula_weight         545.85

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_Int_Tables_number      14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   12.5688(15)
_cell_length_b                   17.320(2)
_cell_length_c                   16.3239(10)
_cell_angle_alpha                90
_cell_angle_beta                 91.481(7)
_cell_angle_gamma                90
_cell_volume                     3552.4(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100.35(10)
_cell_measurement_reflns_used    1361
_cell_measurement_theta_min      5.137
_cell_measurement_theta_max      51.507

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_size_max          0.184
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.108
_exptl_crystal_density_diffrn    1.021
_exptl_crystal_F_000             1208
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
3 5 3 0.0621
-4 -6 -5 0.0461
0 4 -5 0.103
2 0 -5 0.0556
-2 0 5 0.0526
0 1 0 0.096
0 -1 0 0.096
-4 5 -1 0.0904
4 -5 1 0.0604

loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.0006 4.9998 2.9841 0.3929 -0.4552 0.2381
-3.6018 -5.9021 -5.1821 -0.5063 0.6559 -0.1875
-0.0041 3.9905 -5.0112 -0.1315 0.1355 0.5601
1.9958 -0.0087 -5.0080 0.1324 0.3887 0.3297
-1.9958 0.0087 5.0080 -0.1324 -0.3887 -0.3297
-0.0001 0.9995 -0.0020 -0.0061 -0.0562 0.0686
0.0001 -0.9995 0.0020 0.0061 0.0562 -0.0686
-4.0002 4.9986 -1.0008 -0.5309 -0.2656 0.3121
4.0002 -4.9986 1.0008 0.5309 0.2656 -0.3121

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    1.473
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
        Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.372
_exptl_absorpt_correction_T_max  1
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 5.039
_oxdiff_exptl_absorpt_empirical_full_min 0.695

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_ambient_temperature      100.35(10)
_diffrn_ambient_environment      N~2~
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_ub_11      0.1198197
_diffrn_orient_matrix_ub_12      -0.0060548
_diffrn_orient_matrix_ub_13      0.0213195
_diffrn_orient_matrix_ub_21      0.0138993
_diffrn_orient_matrix_ub_22      -0.0564198
_diffrn_orient_matrix_ub_23      -0.0719723
_diffrn_orient_matrix_ub_31      0.0219639
_diffrn_orient_matrix_ub_32      0.0685723
_diffrn_orient_matrix_ub_33      -0.0571908
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0837
_diffrn_reflns_av_unetI/netI     0.0834
_diffrn_reflns_number            33362
_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       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.722
_diffrn_reflns_theta_max         73.993
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_reflns_Friedel_coverage         0
_reflns_number_total             7138
_reflns_number_gt                5803
_reflns_threshold_expression     'I > 2σ(I)'
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -93.00  -7.00   1.00    0.25    --  -21.00 -52.00  11.00   86
  2  ω    -34.00  52.00   1.00    0.25    --  -21.00  52.00 156.00   86
  3  ω     35.00 121.00   1.00    0.25    --   47.89  52.00 156.00   86
  4  ω    -23.00  56.00   1.00    0.25    --   47.89 -52.00  11.00   79
  5  ω    100.00 171.00   1.00    1.00    --  112.88  52.00 156.00   71
  6  ω     35.00  96.00   1.00    0.25    --   47.89-125.00 -60.00   61
  7  ω    -26.00  23.00   1.00    0.25    --   47.89 -19.00-150.00   49
  8  ω     36.00 121.00   1.00    0.25    --   47.89  38.00-120.00   85
  9  ω     35.00  96.00   1.00    0.25    --   47.89-125.00-150.00   61
 10  ω    100.00 171.00   1.00    1.00    --  112.88  15.00-120.00   71
 11  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00 120.00   26
 12  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00  90.00   26
 13  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00  60.00   26
 14  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00-150.00   26
 15  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00  30.00   26
 16  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00 -90.00   26
 17  ω     97.00 171.00   1.00    1.00    --  112.88  61.00 -90.00   74
 18  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00 -60.00   26
 19  ω     42.00 102.00   1.00    1.00    --  112.88 -77.00-180.00   60
 20  ω     91.00 171.00   1.00    1.00    --  112.88  77.00-120.00   80
 21  ω     42.00 102.00   1.00    1.00    --  112.88 -77.00 -30.00   60
 22  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00-120.00   26
 23  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00   0.00   26
 24  ω    100.00 171.00   1.00    1.00    --  112.88  15.00  30.00   71
 25  ω     42.00 106.00   1.00    1.00    --  112.88 -94.00 120.00   64
 26  ω     42.00 102.00   1.00    1.00    --  112.88 -77.00 120.00   60
 27  ω     42.00  68.00   1.00    1.00    --  112.88 -61.00 150.00   26
 28  ω     97.00 171.00   1.00    1.00    --  112.88  61.00  60.00   74
 29  ω     26.00  86.00   1.00    0.25    --   47.89  77.00 -30.00   60
;

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT 2014/4 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     dual
_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_shelx_SHELXL_version_number     2018/3
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1039P)²+4.8802P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_coef       0.0007(2)
_refine_ls_number_reflns         7138
_refine_ls_number_parameters     387
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0875
_refine_ls_R_factor_gt           0.0727
_refine_ls_wR_factor_ref         0.2101
_refine_ls_wR_factor_gt          0.1906
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.062
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.587
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.108

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#

_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. Others
 Sof(Si3B)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C28B)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=Sof(C29B)=Sof(H29D)=Sof(H29E)=Sof(H29F)=1-FVAR(1)
 Sof(Si3A)=Sof(C28A)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29A)=Sof(H29A)=
 Sof(H29B)=Sof(H29C)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
3.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C10(H10A,H10B), C11(H11A,H11B), C15(H15A,H15B), C14(H14A,H14B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C2(H2), C6(H6), C4(H4)
3.c Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C13(H13A,H13B,H13C), C25(H25A,H25B,
 H25C), C8(H8A,H8B,H8C), C7(H7A,H7B,H7C), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C),
 C28A(H28A,H28B,H28C), C29A(H29A,H29B,H29C), C30A(H30A,H30B,H30C), C30B(H30D,
 H30E,H30F), C28B(H28D,H28E,H28F), C29B(H29D,H29E,H29F)
;

#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.009 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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
Si2 Si 0.38837(6) 0.27300(5) 0.58193(5) 0.0305(2) Uani 1 1 d . . . . .
Si3A Si 0.3999(3) 0.5346(2) 0.76700(17) 0.0276(5) Uani 0.813(7) 1 d . . P A 1
Si1 Si 0.37477(7) 0.29765(6) 0.89510(5) 0.0389(3) Uani 1 1 d . . . . .
Na1 Na 0.76200(9) 0.41527(6) 0.74038(7) 0.0311(3) Uani 1 1 d . . . . .
N16 N 0.7839(2) 0.48710(16) 0.61029(16) 0.0372(6) Uani 1 1 d . . . . .
N9 N 0.8200(2) 0.48421(15) 0.86461(15) 0.0349(6) Uani 1 1 d . . . . .
N12 N 0.9594(2) 0.43189(16) 0.72530(17) 0.0385(6) Uani 1 1 d . . . . .
C1 C 0.5845(2) 0.31762(16) 0.74124(17) 0.0282(6) Uani 1 1 d . . . . .
C5 C 0.7289(3) 0.26925(19) 0.8317(2) 0.0380(7) Uani 1 1 d . . . . .
H5 H 0.75611 0.261481 0.8859 0.046 Uiso 1 1 calc R U . . .
C3 C 0.7456(3) 0.25715(19) 0.6868(2) 0.0369(7) Uani 1 1 d . . . . .
H3 H 0.78492 0.242 0.640588 0.044 Uiso 1 1 calc R U . . .
C2 C 0.6462(2) 0.29192(17) 0.67550(18) 0.0314(6) Uani 1 1 d . . . . .
H2 H 0.61882 0.298612 0.621174 0.038 Uiso 1 1 calc R U . . .
C27 C 0.5035(2) 0.45679(16) 0.75812(17) 0.0279(6) Uani 1 1 d . . . . .
C23 C 0.4311(3) 0.36500(16) 0.63235(17) 0.0312(6) Uani 1 1 d . . . . .
H23A H 0.489476 0.386595 0.599796 0.037 Uiso 1 1 calc R U . . .
H23B H 0.370705 0.401473 0.627049 0.037 Uiso 1 1 calc R U . . .
C6 C 0.6320(2) 0.30480(18) 0.81905(18) 0.0330(6) Uani 1 1 d . . . . .
H6 H 0.59484 0.321743 0.865709 0.04 Uiso 1 1 calc R U . . .
C19 C 0.3742(2) 0.33035(18) 0.78619(18) 0.0324(6) Uani 1 1 d . . . . .
C24 C 0.2390(2) 0.26894(19) 0.57122(19) 0.0354(6) Uani 1 1 d . . . . .
H24A H 0.207864 0.273535 0.625435 0.053 Uiso 1 1 calc R U . . .
H24B H 0.217575 0.219653 0.546339 0.053 Uiso 1 1 calc R U . . .
H24C H 0.213707 0.31153 0.536301 0.053 Uiso 1 1 calc R U . . .
C4 C 0.7872(3) 0.24459(19) 0.7650(2) 0.0391(7) Uani 1 1 d . . . . .
H4 H 0.854003 0.219714 0.773127 0.047 Uiso 1 1 calc R U . . .
C26 C 0.4466(3) 0.2671(2) 0.4771(2) 0.0417(8) Uani 1 1 d . . . . .
H26A H 0.419775 0.310075 0.443374 0.062 Uiso 1 1 calc R U . . .
H26B H 0.425892 0.218073 0.451251 0.062 Uiso 1 1 calc R U . . .
H26C H 0.524331 0.270068 0.481961 0.062 Uiso 1 1 calc R U . . .
C10 C 0.9369(3) 0.4763(2) 0.8681(2) 0.0432(8) Uani 1 1 d . . . . .
H10A H 0.954918 0.423927 0.888214 0.052 Uiso 1 1 calc R U . . .
H10B H 0.966073 0.513777 0.908598 0.052 Uiso 1 1 calc R U . . .
C13 C 1.0218(3) 0.3606(2) 0.7360(2) 0.0465(8) Uani 1 1 d . . . . .
H13A H 1.011263 0.339838 0.791066 0.07 Uiso 1 1 calc R U . . .
H13B H 1.097431 0.372008 0.729163 0.07 Uiso 1 1 calc R U . . .
H13C H 0.998306 0.322537 0.695024 0.07 Uiso 1 1 calc R U . . .
B1 B 0.4722(3) 0.36611(18) 0.73014(18) 0.0269(6) Uani 1 1 d . . . . .
C25 C 0.4284(3) 0.18047(19) 0.6354(2) 0.0487(9) Uani 1 1 d . . . . .
H25A H 0.506154 0.176691 0.638391 0.073 Uiso 1 1 calc R U . . .
H25B H 0.399169 0.136373 0.604638 0.073 Uiso 1 1 calc R U . . .
H25C H 0.400507 0.180287 0.690915 0.073 Uiso 1 1 calc R U . . .
C11 C 0.9911(3) 0.4890(2) 0.7877(2) 0.0436(8) Uani 1 1 d . . . . .
H11A H 0.97348 0.541366 0.767088 0.052 Uiso 1 1 calc R U . . .
H11B H 1.069148 0.486449 0.797112 0.052 Uiso 1 1 calc R U . . .
C8 C 0.7889(3) 0.5647(2) 0.8519(2) 0.0491(8) Uani 1 1 d . . . . .
H8A H 0.814243 0.58243 0.798845 0.074 Uiso 1 1 calc R U . . .
H8B H 0.820471 0.596608 0.895726 0.074 Uiso 1 1 calc R U . . .
H8C H 0.711199 0.568949 0.852614 0.074 Uiso 1 1 calc R U . . .
C15 C 0.8907(3) 0.5192(2) 0.6137(2) 0.0475(8) Uani 1 1 d . . . . .
H15A H 0.891532 0.564092 0.651226 0.057 Uiso 1 1 calc R U . . .
H15B H 0.908121 0.538308 0.55848 0.057 Uiso 1 1 calc R U . . .
C7 C 0.7760(3) 0.4566(2) 0.9407(2) 0.0495(9) Uani 1 1 d . . . . .
H7A H 0.698123 0.459515 0.937112 0.074 Uiso 1 1 calc R U . . .
H7B H 0.802272 0.488837 0.986269 0.074 Uiso 1 1 calc R U . . .
H7C H 0.797864 0.402992 0.950079 0.074 Uiso 1 1 calc R U . . .
C14 C 0.9762(3) 0.4636(2) 0.6418(2) 0.0478(8) Uani 1 1 d . . . . .
H14A H 0.978963 0.420257 0.602328 0.057 Uiso 1 1 calc R U . . .
H14B H 1.045855 0.490285 0.641394 0.057 Uiso 1 1 calc R U . . .
C17 C 0.7733(3) 0.4284(2) 0.5443(2) 0.0501(9) Uani 1 1 d . . . . .
H17A H 0.814758 0.3825 0.559699 0.075 Uiso 1 1 calc R U . . .
H17B H 0.800016 0.449805 0.493204 0.075 Uiso 1 1 calc R U . . .
H17C H 0.698266 0.414269 0.53652 0.075 Uiso 1 1 calc R U . . .
C18 C 0.7051(4) 0.5480(2) 0.5923(2) 0.0533(9) Uani 1 1 d . . . . .
H18A H 0.6334 0.525675 0.591728 0.08 Uiso 1 1 calc R U . . .
H18B H 0.718811 0.570661 0.538556 0.08 Uiso 1 1 calc R U . . .
H18C H 0.710538 0.588117 0.634451 0.08 Uiso 1 1 calc R U . . .
C20 C 0.4386(3) 0.3624(3) 0.9746(2) 0.0563(10) Uani 1 1 d . . . . .
H20A H 0.516199 0.357989 0.972189 0.084 Uiso 1 1 calc R U . . .
H20B H 0.415495 0.347061 1.029079 0.084 Uiso 1 1 calc R U . . .
H20C H 0.417425 0.416018 0.96388 0.084 Uiso 1 1 calc R U . . .
C22 C 0.4377(4) 0.1985(3) 0.9056(3) 0.0627(11) Uani 1 1 d . . . . .
H22A H 0.392259 0.160234 0.877706 0.094 Uiso 1 1 calc R U . . .
H22B H 0.445558 0.185116 0.963802 0.094 Uiso 1 1 calc R U . . .
H22C H 0.507903 0.198948 0.880823 0.094 Uiso 1 1 calc R U . . .
C21 C 0.2328(3) 0.2861(3) 0.9266(3) 0.0600(11) Uani 1 1 d . . . . .
H21A H 0.196598 0.336155 0.923351 0.09 Uiso 1 1 calc R U . . .
H21B H 0.231418 0.266812 0.983032 0.09 Uiso 1 1 calc R U . . .
H21C H 0.196388 0.24929 0.889931 0.09 Uiso 1 1 calc R U . . .
C28A C 0.4643(4) 0.6326(3) 0.7643(3) 0.0407(10) Uani 0.813(7) 1 d . . P A 1
H28A H 0.51757 0.636682 0.808956 0.061 Uiso 0.813(7) 1 calc R U P A 1
H28B H 0.409964 0.672569 0.770742 0.061 Uiso 0.813(7) 1 calc R U P A 1
H28C H 0.498887 0.639606 0.711658 0.061 Uiso 0.813(7) 1 calc R U P A 1
C29A C 0.3298(4) 0.5304(2) 0.8672(3) 0.0429(11) Uani 0.813(7) 1 d . . P A 1
H29A H 0.290342 0.481743 0.870735 0.064 Uiso 0.813(7) 1 calc R U P A 1
H29B H 0.280189 0.573847 0.870653 0.064 Uiso 0.813(7) 1 calc R U P A 1
H29C H 0.382313 0.533379 0.912544 0.064 Uiso 0.813(7) 1 calc R U P A 1
C30A C 0.2949(4) 0.5362(2) 0.6838(3) 0.0441(11) Uani 0.813(7) 1 d . . P A 1
H30A H 0.328396 0.543222 0.630741 0.066 Uiso 0.813(7) 1 calc R U P A 1
H30B H 0.245695 0.578957 0.693294 0.066 Uiso 0.813(7) 1 calc R U P A 1
H30C H 0.255721 0.487307 0.683721 0.066 Uiso 0.813(7) 1 calc R U P A 1
Si3B Si 0.4167(15) 0.5362(11) 0.7456(11) 0.048(4) Uani 0.187(7) 1 d . . P A 2
C30B C 0.4221(19) 0.5786(11) 0.6400(14) 0.054(6) Uani 0.187(7) 1 d . . P A 2
H30D H 0.486043 0.610635 0.635913 0.081 Uiso 0.187(7) 1 calc R U P A 2
H30E H 0.358779 0.610458 0.629413 0.081 Uiso 0.187(7) 1 calc R U P A 2
H30F H 0.424355 0.536921 0.59948 0.081 Uiso 0.187(7) 1 calc R U P A 2
C28B C 0.455(2) 0.6132(15) 0.816(2) 0.072(9) Uani 0.187(7) 1 d . . P A 2
H28D H 0.444548 0.596019 0.872299 0.108 Uiso 0.187(7) 1 calc R U P A 2
H28E H 0.410463 0.658694 0.804535 0.108 Uiso 0.187(7) 1 calc R U P A 2
H28F H 0.529734 0.626312 0.808581 0.108 Uiso 0.187(7) 1 calc R U P A 2
C29B C 0.2714(16) 0.5171(12) 0.7658(18) 0.061(7) Uani 0.187(7) 1 d . . P A 2
H29D H 0.246078 0.474009 0.731563 0.092 Uiso 0.187(7) 1 calc R U P A 2
H29E H 0.229496 0.56337 0.752646 0.092 Uiso 0.187(7) 1 calc R U P A 2
H29F H 0.263279 0.503916 0.823714 0.092 Uiso 0.187(7) 1 calc R U P A 2
H19A H 0.317(3) 0.367(3) 0.781(2) 0.049(11) Uiso 1 1 d . . . . .
H19B H 0.347(4) 0.280(3) 0.755(3) 0.063(13) Uiso 1 1 d . . . . .
H27A H 0.556(3) 0.474(2) 0.723(2) 0.028(8) Uiso 1 1 d . . . . .
H27B H 0.535(3) 0.461(2) 0.816(2) 0.033(9) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
Si2 C23 1.866(3) . ?
Si2 C24 1.883(3) . ?
Si2 C26 1.882(3) . ?
Si2 C25 1.887(4) . ?
Si3A C27 1.882(5) . ?
Si3A C28A 1.882(6) . ?
Si3A C29A 1.879(5) . ?
Si3A C30A 1.869(6) . ?
Si1 C19 1.866(3) . ?
Si1 C20 1.879(4) . ?
Si1 C22 1.897(4) . ?
Si1 C21 1.881(4) . ?
Na1 N16 2.483(3) . ?
Na1 N9 2.448(3) . ?
Na1 N12 2.516(3) . ?
Na1 C1 2.800(3) . ?
Na1 C5 2.971(3) . ?
Na1 C3 2.881(3) . ?
Na1 C2 2.779(3) . ?
Na1 C6 2.844(3) . ?
Na1 C4 2.999(3) . ?
N16 C15 1.454(5) . ?
N16 C17 1.484(4) . ?
N16 C18 1.471(5) . ?
N9 C10 1.475(5) . ?
N9 C8 1.460(4) . ?
N9 C7 1.454(4) . ?
N12 C13 1.470(4) . ?
N12 C11 1.468(4) . ?
N12 C14 1.490(5) . ?
C1 C2 1.412(4) . ?
C1 C6 1.407(4) . ?
C1 B1 1.648(4) . ?
C5 H5 0.95 . ?
C5 C6 1.376(4) . ?
C5 C4 1.394(5) . ?
C3 H3 0.95 . ?
C3 C2 1.394(4) . ?
C3 C4 1.385(5) . ?
C2 H2 0.95 . ?
C27 B1 1.680(4) . ?
C27 Si3B 1.76(2) . ?
C27 H27A 0.94(4) . ?
C27 H27B 1.01(4) . ?
C23 H23A 0.99 . ?
C23 H23B 0.99 . ?
C23 B1 1.665(4) . ?
C6 H6 0.95 . ?
C19 B1 1.673(4) . ?
C19 H19A 0.96(5) . ?
C19 H19B 1.06(5) . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C4 H4 0.95 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
C10 H10A 0.99 . ?
C10 H10B 0.99 . ?
C10 C11 1.510(5) . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C11 H11A 0.99 . ?
C11 H11B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C15 C14 1.505(6) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C17 H17A 0.98 . ?
C17 H17B 0.98 . ?
C17 H17C 0.98 . ?
C18 H18A 0.98 . ?
C18 H18B 0.98 . ?
C18 H18C 0.98 . ?
C20 H20A 0.98 . ?
C20 H20B 0.98 . ?
C20 H20C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C28A H28A 0.98 . ?
C28A H28B 0.98 . ?
C28A H28C 0.98 . ?
C29A H29A 0.98 . ?
C29A H29B 0.98 . ?
C29A H29C 0.98 . ?
C30A H30A 0.98 . ?
C30A H30B 0.98 . ?
C30A H30C 0.98 . ?
Si3B C30B 1.88(3) . ?
Si3B C28B 1.81(3) . ?
Si3B C29B 1.89(3) . ?
C30B H30D 0.98 . ?
C30B H30E 0.98 . ?
C30B H30F 0.98 . ?
C28B H28D 0.98 . ?
C28B H28E 0.98 . ?
C28B H28F 0.98 . ?
C29B H29D 0.98 . ?
C29B H29E 0.98 . ?
C29B H29F 0.98 . ?

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
C23 Si2 C24 110.37(14) . . ?
C23 Si2 C26 109.47(15) . . ?
C23 Si2 C25 116.81(14) . . ?
C24 Si2 C25 105.33(16) . . ?
C26 Si2 C24 108.89(14) . . ?
C26 Si2 C25 105.64(18) . . ?
C28A Si3A C27 110.2(2) . . ?
C29A Si3A C27 112.4(2) . . ?
C29A Si3A C28A 105.5(3) . . ?
C30A Si3A C27 115.6(2) . . ?
C30A Si3A C28A 105.4(3) . . ?
C30A Si3A C29A 107.2(3) . . ?
C19 Si1 C20 117.89(18) . . ?
C19 Si1 C22 110.65(19) . . ?
C19 Si1 C21 108.21(17) . . ?
C20 Si1 C22 108.0(2) . . ?
C20 Si1 C21 105.4(2) . . ?
C21 Si1 C22 106.0(2) . . ?
N16 Na1 N12 74.20(10) . . ?
N16 Na1 C1 114.38(10) . . ?
N16 Na1 C5 151.16(10) . . ?
N16 Na1 C3 103.03(10) . . ?
N16 Na1 C2 97.34(10) . . ?
N16 Na1 C6 143.22(10) . . ?
N16 Na1 C4 126.53(10) . . ?
N9 Na1 N16 115.28(10) . . ?
N9 Na1 N12 75.65(10) . . ?
N9 Na1 C1 120.71(10) . . ?
N9 Na1 C5 92.42(10) . . ?
N9 Na1 C3 137.11(10) . . ?
N9 Na1 C2 146.34(10) . . ?
N9 Na1 C6 96.68(10) . . ?
N9 Na1 C4 109.97(10) . . ?
N12 Na1 C1 149.03(10) . . ?
N12 Na1 C5 107.33(10) . . ?
N12 Na1 C3 98.18(10) . . ?
N12 Na1 C2 123.96(10) . . ?
N12 Na1 C6 134.48(10) . . ?
N12 Na1 C4 91.43(10) . . ?
C1 Na1 C5 50.30(9) . . ?
C1 Na1 C3 51.41(9) . . ?
C1 Na1 C6 28.86(8) . . ?
C1 Na1 C4 59.02(9) . . ?
C5 Na1 C4 27.01(10) . . ?
C3 Na1 C5 48.16(10) . . ?
C3 Na1 C4 27.14(9) . . ?
C2 Na1 C1 29.32(9) . . ?
C2 Na1 C5 57.18(9) . . ?
C2 Na1 C3 28.45(9) . . ?
C2 Na1 C6 49.73(9) . . ?
C2 Na1 C4 49.15(9) . . ?
C6 Na1 C5 27.26(9) . . ?
C6 Na1 C3 57.31(9) . . ?
C6 Na1 C4 48.41(9) . . ?
C15 N16 Na1 106.3(2) . . ?
C15 N16 C17 110.8(3) . . ?
C15 N16 C18 110.5(3) . . ?
C17 N16 Na1 105.5(2) . . ?
C18 N16 Na1 116.2(2) . . ?
C18 N16 C17 107.4(3) . . ?
C10 N9 Na1 105.16(18) . . ?
C8 N9 Na1 106.0(2) . . ?
C8 N9 C10 110.8(3) . . ?
C7 N9 Na1 115.9(2) . . ?
C7 N9 C10 109.7(3) . . ?
C7 N9 C8 109.2(3) . . ?
C13 N12 Na1 114.6(2) . . ?
C13 N12 C14 109.3(3) . . ?
C11 N12 Na1 105.0(2) . . ?
C11 N12 C13 110.4(3) . . ?
C11 N12 C14 110.1(3) . . ?
C14 N12 Na1 107.2(2) . . ?
C2 C1 Na1 74.53(16) . . ?
C2 C1 B1 124.2(2) . . ?
C6 C1 Na1 77.31(17) . . ?
C6 C1 C2 114.1(3) . . ?
C6 C1 B1 121.4(3) . . ?
B1 C1 Na1 111.82(17) . . ?
Na1 C5 H5 122.4 . . ?
C6 C5 Na1 71.25(18) . . ?
C6 C5 H5 120 . . ?
C6 C5 C4 120.1(3) . . ?
C4 C5 Na1 77.64(19) . . ?
C4 C5 H5 120 . . ?
Na1 C3 H3 118 . . ?
C2 C3 Na1 71.74(17) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 Na1 81.21(19) . . ?
C4 C3 H3 119.8 . . ?
C4 C3 C2 120.4(3) . . ?
Na1 C2 H2 115.8 . . ?
C1 C2 Na1 76.15(16) . . ?
C1 C2 H2 118.6 . . ?
C3 C2 Na1 79.81(18) . . ?
C3 C2 C1 122.9(3) . . ?
C3 C2 H2 118.6 . . ?
Si3A C27 H27A 108(2) . . ?
Si3A C27 H27B 98(2) . . ?
B1 C27 Si3A 122.2(2) . . ?
B1 C27 Si3B 123.9(7) . . ?
B1 C27 H27A 107(2) . . ?
B1 C27 H27B 113(2) . . ?
Si3B C27 H27A 97(2) . . ?
Si3B C27 H27B 106(2) . . ?
H27A C27 H27B 107(3) . . ?
Si2 C23 H23A 107.1 . . ?
Si2 C23 H23B 107.1 . . ?
H23A C23 H23B 106.8 . . ?
B1 C23 Si2 120.75(19) . . ?
B1 C23 H23A 107.1 . . ?
B1 C23 H23B 107.1 . . ?
Na1 C6 H6 117 . . ?
C1 C6 Na1 73.83(16) . . ?
C1 C6 H6 118 . . ?
C5 C6 Na1 81.49(19) . . ?
C5 C6 C1 124.0(3) . . ?
C5 C6 H6 118 . . ?
Si1 C19 H19A 106(2) . . ?
Si1 C19 H19B 102(3) . . ?
B1 C19 Si1 130.4(2) . . ?
B1 C19 H19A 105(3) . . ?
B1 C19 H19B 106(3) . . ?
H19A C19 H19B 106(4) . . ?
Si2 C24 H24A 109.5 . . ?
Si2 C24 H24B 109.5 . . ?
Si2 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Na1 C4 H4 123.7 . . ?
C5 C4 Na1 75.35(19) . . ?
C5 C4 H4 120.7 . . ?
C3 C4 Na1 71.65(18) . . ?
C3 C4 C5 118.5(3) . . ?
C3 C4 H4 120.7 . . ?
Si2 C26 H26A 109.5 . . ?
Si2 C26 H26B 109.5 . . ?
Si2 C26 H26C 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N9 C10 H10A 108.5 . . ?
N9 C10 H10B 108.5 . . ?
N9 C10 C11 115.1(3) . . ?
H10A C10 H10B 107.5 . . ?
C11 C10 H10A 108.5 . . ?
C11 C10 H10B 108.5 . . ?
N12 C13 H13A 109.5 . . ?
N12 C13 H13B 109.5 . . ?
N12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C1 B1 C27 104.6(2) . . ?
C1 B1 C23 110.1(2) . . ?
C1 B1 C19 113.1(2) . . ?
C23 B1 C27 109.6(2) . . ?
C23 B1 C19 107.8(2) . . ?
C19 B1 C27 111.6(2) . . ?
Si2 C25 H25A 109.5 . . ?
Si2 C25 H25B 109.5 . . ?
Si2 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N12 C11 C10 112.6(3) . . ?
N12 C11 H11A 109.1 . . ?
N12 C11 H11B 109.1 . . ?
C10 C11 H11A 109.1 . . ?
C10 C11 H11B 109.1 . . ?
H11A C11 H11B 107.8 . . ?
N9 C8 H8A 109.5 . . ?
N9 C8 H8B 109.5 . . ?
N9 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N16 C15 H15A 108.6 . . ?
N16 C15 H15B 108.6 . . ?
N16 C15 C14 114.8(3) . . ?
H15A C15 H15B 107.6 . . ?
C14 C15 H15A 108.6 . . ?
C14 C15 H15B 108.6 . . ?
N9 C7 H7A 109.5 . . ?
N9 C7 H7B 109.5 . . ?
N9 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N12 C14 C15 113.4(3) . . ?
N12 C14 H14A 108.9 . . ?
N12 C14 H14B 108.9 . . ?
C15 C14 H14A 108.9 . . ?
C15 C14 H14B 108.9 . . ?
H14A C14 H14B 107.7 . . ?
N16 C17 H17A 109.5 . . ?
N16 C17 H17B 109.5 . . ?
N16 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N16 C18 H18A 109.5 . . ?
N16 C18 H18B 109.5 . . ?
N16 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C20 H20A 109.5 . . ?
Si1 C20 H20B 109.5 . . ?
Si1 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
Si1 C22 H22A 109.5 . . ?
Si1 C22 H22B 109.5 . . ?
Si1 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si1 C21 H21A 109.5 . . ?
Si1 C21 H21B 109.5 . . ?
Si1 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3A C28A H28A 109.5 . . ?
Si3A C28A H28B 109.5 . . ?
Si3A C28A H28C 109.5 . . ?
H28A C28A H28B 109.5 . . ?
H28A C28A H28C 109.5 . . ?
H28B C28A H28C 109.5 . . ?
Si3A C29A H29A 109.5 . . ?
Si3A C29A H29B 109.5 . . ?
Si3A C29A H29C 109.5 . . ?
H29A C29A H29B 109.5 . . ?
H29A C29A H29C 109.5 . . ?
H29B C29A H29C 109.5 . . ?
Si3A C30A H30A 109.5 . . ?
Si3A C30A H30B 109.5 . . ?
Si3A C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C27 Si3B C30B 112.0(11) . . ?
C27 Si3B C28B 110.3(15) . . ?
C27 Si3B C29B 116.1(12) . . ?
C30B Si3B C29B 106.7(15) . . ?
C28B Si3B C30B 106.1(18) . . ?
C28B Si3B C29B 104.9(16) . . ?
Si3B C30B H30D 109.5 . . ?
Si3B C30B H30E 109.5 . . ?
Si3B C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
Si3B C28B H28D 109.5 . . ?
Si3B C28B H28E 109.5 . . ?
Si3B C28B H28F 109.5 . . ?
H28D C28B H28E 109.5 . . ?
H28D C28B H28F 109.5 . . ?
H28E C28B H28F 109.5 . . ?
Si3B C29B H29D 109.5 . . ?
Si3B C29B H29E 109.5 . . ?
Si3B C29B H29F 109.5 . . ?
H29D C29B H29E 109.5 . . ?
H29D C29B H29F 109.5 . . ?
H29E C29B H29F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Si2 C23 B1 C1 66.2(3) . . . . ?
Si2 C23 B1 C27 -179.2(2) . . . . ?
Si2 C23 B1 C19 -57.6(3) . . . . ?
Si3A C27 B1 C1 -173.7(2) . . . . ?
Si3A C27 B1 C23 68.3(3) . . . . ?
Si3A C27 B1 C19 -51.1(3) . . . . ?
Si1 C19 B1 C1 44.9(4) . . . . ?
Si1 C19 B1 C27 -72.8(3) . . . . ?
Si1 C19 B1 C23 166.8(2) . . . . ?
Na1 N16 C15 C14 46.0(3) . . . . ?
Na1 N9 C10 C11 44.0(3) . . . . ?
Na1 N12 C11 C10 41.3(3) . . . . ?
Na1 N12 C14 C15 35.7(3) . . . . ?
Na1 C1 C2 C3 67.9(3) . . . . ?
Na1 C1 C6 C5 -67.6(3) . . . . ?
Na1 C1 B1 C27 -21.0(2) . . . . ?
Na1 C1 B1 C23 96.7(2) . . . . ?
Na1 C1 B1 C19 -142.67(19) . . . . ?
Na1 C5 C6 C1 63.9(3) . . . . ?
Na1 C5 C4 C3 -59.2(3) . . . . ?
Na1 C3 C2 C1 -66.1(3) . . . . ?
Na1 C3 C4 C5 61.1(3) . . . . ?
N16 C15 C14 N12 -59.3(4) . . . . ?
N9 C10 C11 N12 -63.0(4) . . . . ?
C2 C1 C6 Na1 66.4(2) . . . . ?
C2 C1 C6 C5 -1.2(4) . . . . ?
C2 C1 B1 C27 -106.7(3) . . . . ?
C2 C1 B1 C23 11.0(4) . . . . ?
C2 C1 B1 C19 131.6(3) . . . . ?
C2 C3 C4 Na1 -62.7(3) . . . . ?
C2 C3 C4 C5 -1.6(5) . . . . ?
C6 C1 C2 Na1 -68.1(2) . . . . ?
C6 C1 C2 C3 -0.2(4) . . . . ?
C6 C1 B1 C27 67.1(3) . . . . ?
C6 C1 B1 C23 -175.1(3) . . . . ?
C6 C1 B1 C19 -54.5(3) . . . . ?
C6 C5 C4 Na1 59.5(3) . . . . ?
C6 C5 C4 C3 0.4(5) . . . . ?
C24 Si2 C23 B1 104.0(2) . . . . ?
C4 C5 C6 Na1 -62.8(3) . . . . ?
C4 C5 C6 C1 1.1(5) . . . . ?
C4 C3 C2 Na1 67.7(3) . . . . ?
C4 C3 C2 C1 1.6(5) . . . . ?
C26 Si2 C23 B1 -136.1(2) . . . . ?
C13 N12 C11 C10 -82.8(4) . . . . ?
C13 N12 C14 C15 160.4(3) . . . . ?
B1 C1 C2 Na1 106.2(3) . . . . ?
B1 C1 C2 C3 174.0(3) . . . . ?
B1 C1 C6 Na1 -108.0(2) . . . . ?
B1 C1 C6 C5 -175.6(3) . . . . ?
B1 C27 Si3B C30B -84.2(13) . . . . ?
B1 C27 Si3B C28B 157.9(15) . . . . ?
B1 C27 Si3B C29B 38.7(16) . . . . ?
C25 Si2 C23 B1 -16.2(3) . . . . ?
C11 N12 C14 C15 -78.1(4) . . . . ?
C8 N9 C10 C11 -70.1(4) . . . . ?
C7 N9 C10 C11 169.3(3) . . . . ?
C14 N12 C11 C10 156.4(3) . . . . ?
C17 N16 C15 C14 -68.1(4) . . . . ?
C18 N16 C15 C14 173.0(3) . . . . ?
C20 Si1 C19 B1 47.5(3) . . . . ?
C22 Si1 C19 B1 -77.4(3) . . . . ?
C21 Si1 C19 B1 166.9(3) . . . . ?
C28A Si3A C27 B1 -161.0(3) . . . . ?
C29A Si3A C27 B1 81.6(3) . . . . ?
C30A Si3A C27 B1 -41.8(4) . . . . ?
Si3B C27 B1 C1 171.5(7) . . . . ?
Si3B C27 B1 C23 53.5(7) . . . . ?
Si3B C27 B1 C19 -65.9(7) . . . . ?

#----------------------------------------------------------------------------#
#                   SHELX RES FILE                                           #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   SHELX HKL FILE                                           #
#----------------------------------------------------------------------------#


# END of CIF
####################################################################### 
# 
# 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_21eh054_lb-17-53
_database_code_depnum_ccdc_archive 'CCDC 2245606'
loop_
_audit_author_name
_audit_author_address
'Lorraine Andrade Malaspina'
;University of Bern
Switzerland
;
_audit_update_record             
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_21eh054_lb-17-53    
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       9.82 Check
RESPONSE: The structure contains substitutional disorder, where one component has moyety formula C31 H59 B N3 Na O2 Si2 and the second component has moyety formula C30 H57 B N3 Na O1 Si2.
;
# Added during the CSD deposition process: Wednesday 01 March 2023 05:25 PM
# end Validation Reply Form

_audit_creation_date             2021-03-07
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C30.67 H58.35 B N3 Na O1.67 Si2'
_chemical_formula_sum            'C31 H59 B N3 Na O2 Si2'
_chemical_formula_weight         595.79
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.1353 0.1239 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   11.64110(10)
_cell_length_b                   18.66620(10)
_cell_length_c                   33.6871(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7320.04(9)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    38757
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      79.649
_cell_measurement_theta_min      2.692
_shelx_estimated_absorpt_T_max   0.700
_shelx_estimated_absorpt_T_min   0.560
_exptl_absorpt_coefficient_mu    1.210
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.88377
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
        CrysAlisPro 1.171.41.99a (Rigaku Oxford Diffraction, 2021)
        Empirical absorption correction using spherical harmonics,
        implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2608
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 1 0 0.2492
-1 -1 0 0.2917
-1 1 0 0.1948
-1 0 0 0.2468
1 0 0 0.235
1 1 -1 0.2455
0 1 -1 0.2367
0 -1 1 0.1736
1 -1 -1 0.1582
-1 1 1 0.1981
0 0 -1 0.1619
0 0 1 0.1555
0 -1 -1 0.1843
0 1 1 0.2379
-1 1 -1 0.1808
1 -1 1 0.1849
1 1 1 0.2403
1 0 1 0.2268
-1 0 -1 0.2427
0 -1 0 0.1649
0 1 0 0.2299
3 4 -19 0.1916
-1 9 -14 0.2159
5 -1 -16 0.1765
-1 -8 17 0.1685
-4 0 18 0.1975
2 -5 19 0.1449
3 -7 -16 0.1629
-2 5 -20 0.2002
-3 6 17 0.2222
4 4 16 0.2136
6 -2 15 0.1865
-5 1 -15 0.2153

_exptl_crystal_size_max          0.542
_exptl_crystal_size_mid          0.374
_exptl_crystal_size_min          0.317
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            57708
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.502
_diffrn_reflns_theta_min         4.617
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 10
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
        List of Runs (angles in degrees, time in seconds):
  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -85.00 -27.00   0.50    0.15    --  -21.00 153.00 -85.00  116
  2  ω    -66.00 -10.00   0.50    0.15    --  -21.00 121.00 115.00  112
  3  ω     32.00  93.00   0.50    0.15    --   47.91-121.00  32.00  122
  4  ω     42.00 110.00   0.50    0.80    --  113.25-121.00  32.00  136
  5  ω     98.00 177.00   0.50    0.80    --  113.25 121.00 115.00  158
  6  ω    -96.00  -7.00   0.50    0.15    --  -21.00 -15.00-180.00  178
  7  ω    -26.00  23.00   0.50    0.15    --   47.91 -19.00  30.00   98
  8  ω    -26.00  23.00   0.50    0.15    --   47.91 -19.00 -60.00   98
  9  ω    -26.00  23.00   0.50    0.15    --   47.91 -19.00  60.00   98
 10  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00  60.00   50
 11  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00 -90.00   50
 12  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00-150.00   50
 13  ω     42.00  67.00   0.50    0.80    --  113.25-125.00 -60.00   50
 14  ω     96.00 139.00   0.50    0.80    --  113.25 125.00   0.00   86
 15  ω     78.00 110.00   0.50    0.80    --  113.25-125.00 -60.00   64
 16  ω     43.00  68.00   0.50    0.80    --  113.25 -61.00  30.00   50
 17  ω     49.00 111.00   0.50    0.80    --  113.25-125.00-120.00  124
 18  ω    101.00 126.00   0.50    0.80    --  113.25  15.00 120.00   50
 19  ω     43.00 106.00   0.50    0.80    --  113.25 -94.00  30.00  126
 20  ω    112.00 162.00   0.50    0.80    --  113.25 125.00 -60.00  100
 21  ω    104.00 157.00   0.50    0.80    --  113.25  77.00 150.00  106
 22  ω     43.00  94.00   0.50    0.80    --  113.25 -94.00-180.00  102
 23  ω     95.00 155.00   0.50    0.80    --  113.25 125.00  60.00  120
 24  ω    146.00 173.00   0.50    0.80    --  113.25 125.00   0.00   54
 25  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00   0.00   50
 26  ω     42.00  67.00   0.50    0.80    --  113.25 -61.00 120.00   50
 27  ω     53.00 102.00   0.50    0.80    --  113.25 -77.00 -60.00   98
 28  ω    101.00 156.00   0.50    0.80    --  113.25  45.00-150.00  110
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7296
_reflns_number_total             7500
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.99a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       0.00024(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         7500
_refine_ls_number_restraints     12
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0459
_refine_ls_restrained_S_all      1.136
_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)+(0.0335P)²+4.6065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1080
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, H5 of C5, H9 of C9, H4 of C4, H2 of C2, H12 of C12, H11
  of C11, H10 of C10, H3 of C3, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, H13 of C13, All C(H,H,H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
Uanis(C21A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N3A) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.02
3. Others
 Sof(C28A)=Sof(H28C)=Sof(H28D)=Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=Sof(H31D)=Sof(H31E)=Sof(H31F)=Sof(N3A)=
 1-FVAR(1)
 Sof(N3)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(C29)=Sof(H29A)=Sof(H29B)=Sof(C31)=
 Sof(H31A)=Sof(H31B)=Sof(H31C)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(H30C)=FVAR(1)
 Sof(H19C)=Sof(H19D)=Sof(H20D)=Sof(H20E)=Sof(H20F)=Sof(C22A)=Sof(H22D)=
 Sof(H22E)=Sof(H22F)=Sof(C21A)=Sof(H21D)=Sof(H21E)=Sof(H21F)=Sof(Si)=1-FVAR(2)
 Sof(Si2)=Sof(H19A)=Sof(H19B)=Sof(H20A)=Sof(H20B)=Sof(H20C)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(2)
 Sof(H13)=1-FVAR(3)
 Sof(O2)=Sof(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=FVAR(3)
4.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C19(H19C,H19D), C15(H15A,H15B), C25(H25A,H25B), C26(H26A,
 H26B), C28(H28A,H28B), C29(H29A,H29B), C28A(H28C,H28D), C29A(H29C,H29D)
4.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C5(H5), C9(H9), C4(H4), C2(H2), C10(H10), C3(H3), C12(H12), C11(H11)
4.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C20(H20A,H20B,H20C), C20(H20D,H20E,
 H20F), C27(H27A,H27B,H27C), C7(H7A,H7B,H7C), C18(H18A,H18B,H18C), C16(H16A,
 H16B,H16C), C17(H17A,H17B,H17C), C31(H31A,H31B,H31C), C30(H30A,H30B,H30C),
 C14(H14A,H14B,H14C), C22(H22A,H22B,H22C), C21(H21A,H21B,H21C), C30A(H30D,H30E,
 H30F), C31A(H31D,H31E,H31F), C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.27874(4) 0.72612(2) 0.44183(2) 0.03090(12) Uani 1 1 d . . . . .
Si2 Si 0.3760(2) 0.77765(13) 0.30539(8) 0.0302(4) Uani 0.699(7) 1 d . . P A 1
Na1 Na 0.70977(5) 0.54808(3) 0.37795(2) 0.02597(14) Uani 1 1 d . . . . .
O1 O 0.60271(9) 0.59887(7) 0.32183(3) 0.0325(3) Uani 1 1 d . . . . .
N1 N 0.90711(12) 0.60209(8) 0.36293(4) 0.0332(3) Uani 1 1 d . . . . .
N3 N 0.6637(3) 0.41788(18) 0.36455(12) 0.0337(7) Uani 0.839(7) 1 d . . P B 1
N2 N 0.86994(12) 0.46672(8) 0.41230(5) 0.0376(3) Uani 1 1 d . . . . .
C1 C 0.40109(12) 0.59909(8) 0.33650(4) 0.0237(3) Uani 1 1 d . . . . .
C8 C 0.51068(13) 0.63502(8) 0.40372(4) 0.0255(3) Uani 1 1 d . . . . .
O2 O 0.40068(14) 0.52885(9) 0.41256(5) 0.0310(5) Uani 0.673(4) 1 d . . P C 1
C19 C 0.45655(13) 0.73762(8) 0.34942(5) 0.0267(3) Uani 1 1 d . . . . .
H19A H 0.5371 0.7307 0.3408 0.032 Uiso 0.699(7) 1 calc R . P A 1
H19B H 0.4578 0.7747 0.3704 0.032 Uiso 0.699(7) 1 calc R . P A 1
H19C H 0.5287 0.7267 0.3351 0.032 Uiso 0.301(7) 1 calc R . P A 2
H19D H 0.4773 0.7708 0.3712 0.032 Uiso 0.301(7) 1 calc R . P A 2
C6 C 0.49169(13) 0.57478(8) 0.31286(4) 0.0262(3) Uani 1 1 d . . . . .
C13 C 0.49707(14) 0.57001(9) 0.42423(5) 0.0295(3) Uani 1 1 d . . . . .
H13 H 0.4356 0.5392 0.4170 0.044 Uiso 0.327(4) 1 calc R . P C 2
C15 C 0.29205(13) 0.67334(8) 0.39507(5) 0.0269(3) Uani 1 1 d . . . . .
H15A H 0.2622 0.6248 0.4010 0.032 Uiso 1 1 calc R . . . .
H15B H 0.2379 0.6951 0.3759 0.032 Uiso 1 1 calc R . . . .
C5 C 0.47805(15) 0.52646(9) 0.28170(5) 0.0328(4) Uani 1 1 d . . . . .
H5 H 0.5424 0.5130 0.2660 0.039 Uiso 1 1 calc R . . . .
C9 C 0.60482(13) 0.67670(9) 0.41545(5) 0.0312(3) Uani 1 1 d . . . . .
H9 H 0.6189 0.7203 0.4018 0.037 Uiso 1 1 calc R . . . .
C4 C 0.37072(16) 0.49812(9) 0.27357(5) 0.0365(4) Uani 1 1 d . . . . .
H4 H 0.3607 0.4651 0.2524 0.044 Uiso 1 1 calc R . . . .
C2 C 0.29487(14) 0.56792(9) 0.32710(5) 0.0319(3) Uani 1 1 d . . . . .
H2 H 0.2299 0.5813 0.3425 0.038 Uiso 1 1 calc R . . . .
C10 C 0.67861(15) 0.65753(10) 0.44606(5) 0.0384(4) Uani 1 1 d . . . . .
H10 H 0.7408 0.6879 0.4532 0.046 Uiso 1 1 calc R . . . .
C3 C 0.27871(16) 0.51852(9) 0.29663(5) 0.0372(4) Uani 1 1 d . . . . .
H3 H 0.2047 0.4990 0.2918 0.045 Uiso 1 1 calc R . . . .
C12 C 0.57047(17) 0.54918(10) 0.45478(5) 0.0392(4) Uani 1 1 d . . . . .
H12 H 0.5592 0.5047 0.4679 0.047 Uiso 1 1 calc R . . . .
C11 C 0.66064(17) 0.59414(11) 0.46599(5) 0.0439(5) Uani 1 1 d . . . . .
H11 H 0.7096 0.5810 0.4874 0.053 Uiso 1 1 calc R . . . .
C23 C 0.90610(17) 0.68036(10) 0.36554(6) 0.0440(4) Uani 1 1 d . . . . .
H23A H 0.8561 0.6999 0.3448 0.066 Uiso 1 1 calc GR . . . .
H23B H 0.9843 0.6987 0.3619 0.066 Uiso 1 1 calc GR . . . .
H23C H 0.8773 0.6949 0.3917 0.066 Uiso 1 1 calc GR . . . .
C25 C 0.98208(14) 0.57455(10) 0.39473(6) 0.0390(4) Uani 1 1 d . . . . .
H25A H 0.9574 0.5955 0.4203 0.047 Uiso 1 1 calc R . . . .
H25B H 1.0618 0.5905 0.3896 0.047 Uiso 1 1 calc R . . . .
C26 C 0.98074(15) 0.49403(11) 0.39823(6) 0.0415(4) Uani 1 1 d . . . . .
H26A H 0.9979 0.4728 0.3720 0.050 Uiso 1 1 calc R . . . .
H26B H 1.0418 0.4788 0.4169 0.050 Uiso 1 1 calc R . . . .
C24 C 0.95201(17) 0.58173(12) 0.32376(6) 0.0458(5) Uani 1 1 d . . . . .
H24A H 0.9481 0.5296 0.3207 0.069 Uiso 1 1 calc GR . . . .
H24B H 1.0320 0.5975 0.3214 0.069 Uiso 1 1 calc GR . . . .
H24C H 0.9058 0.6046 0.3030 0.069 Uiso 1 1 calc GR . . . .
C20 C 0.44853(19) 0.86326(10) 0.29200(6) 0.0473(5) Uani 1 1 d . . . . .
H20A H 0.4146 0.8824 0.2676 0.071 Uiso 0.699(7) 1 calc GR . P A 1
H20B H 0.5306 0.8545 0.2878 0.071 Uiso 0.699(7) 1 calc GR . P A 1
H20C H 0.4386 0.8979 0.3136 0.071 Uiso 0.699(7) 1 calc GR . P A 1
H20D H 0.4775 0.8961 0.3124 0.071 Uiso 0.301(7) 1 calc GR . P A 2
H20E H 0.3956 0.8890 0.2744 0.071 Uiso 0.301(7) 1 calc GR . P A 2
H20F H 0.5131 0.8446 0.2764 0.071 Uiso 0.301(7) 1 calc GR . P A 2
B1 B 0.41535(14) 0.66173(9) 0.37087(5) 0.0231(3) Uani 1 1 d . . . . .
C27 C 0.86749(18) 0.46884(11) 0.45557(6) 0.0485(5) Uani 1 1 d . . . . .
H27A H 0.8823 0.5179 0.4646 0.073 Uiso 1 1 calc GR . . . .
H27B H 0.9267 0.4368 0.4662 0.073 Uiso 1 1 calc GR . . . .
H27C H 0.7918 0.4533 0.4650 0.073 Uiso 1 1 calc GR . . . .
C28 C 0.8521(3) 0.3934(2) 0.39662(12) 0.0426(8) Uani 0.839(7) 1 d . . P B 1
H28A H 0.8903 0.3585 0.4143 0.051 Uiso 0.839(7) 1 calc R . P B 1
H28B H 0.8879 0.3896 0.3700 0.051 Uiso 0.839(7) 1 calc R . P B 1
C7 C 0.66189(17) 0.63097(15) 0.28940(6) 0.0583(6) Uani 1 1 d . . . . .
H7A H 0.7246 0.6609 0.2995 0.087 Uiso 1 1 calc GR . . . .
H7B H 0.6084 0.6607 0.2741 0.087 Uiso 1 1 calc GR . . . .
H7C H 0.6935 0.5934 0.2722 0.087 Uiso 1 1 calc GR . . . .
C18 C 0.12358(16) 0.74592(15) 0.45133(7) 0.0600(7) Uani 1 1 d . . . . .
H18A H 0.0922 0.7735 0.4291 0.090 Uiso 1 1 calc GR . . . .
H18B H 0.1162 0.7738 0.4759 0.090 Uiso 1 1 calc GR . . . .
H18C H 0.0811 0.7008 0.4540 0.090 Uiso 1 1 calc GR . . . .
C16 C 0.3335(2) 0.67506(13) 0.48591(6) 0.0593(6) Uani 1 1 d . . . . .
H16A H 0.2984 0.6274 0.4864 0.089 Uiso 1 1 calc GR . . . .
H16B H 0.3137 0.7009 0.5103 0.089 Uiso 1 1 calc GR . . . .
H16C H 0.4172 0.6703 0.4840 0.089 Uiso 1 1 calc GR . . . .
C17 C 0.3572(2) 0.81327(11) 0.44286(7) 0.0606(7) Uani 1 1 d . . . . .
H17A H 0.4398 0.8045 0.4404 0.091 Uiso 1 1 calc GR . . . .
H17B H 0.3416 0.8378 0.4680 0.091 Uiso 1 1 calc GR . . . .
H17C H 0.3312 0.8433 0.4207 0.091 Uiso 1 1 calc GR . . . .
C29 C 0.7255(3) 0.37510(11) 0.39349(9) 0.0439(8) Uani 0.839(7) 1 d . . P B 1
H29A H 0.7178 0.3239 0.3863 0.053 Uiso 0.839(7) 1 calc R . P B 1
H29B H 0.6893 0.3818 0.4198 0.053 Uiso 0.839(7) 1 calc R . P B 1
C31 C 0.5410(3) 0.39976(15) 0.36605(12) 0.0492(8) Uani 0.839(7) 1 d . . P B 1
H31A H 0.5121 0.4071 0.3931 0.074 Uiso 0.839(7) 1 calc GR . P B 1
H31B H 0.5304 0.3495 0.3584 0.074 Uiso 0.839(7) 1 calc GR . P B 1
H31C H 0.4986 0.4306 0.3476 0.074 Uiso 0.839(7) 1 calc GR . P B 1
C30 C 0.7055(4) 0.4045(4) 0.3237(2) 0.0532(12) Uani 0.839(7) 1 d . . P B 1
H30A H 0.6561 0.4297 0.3047 0.080 Uiso 0.839(7) 1 calc GR . P B 1
H30B H 0.7035 0.3530 0.3181 0.080 Uiso 0.839(7) 1 calc GR . P B 1
H30C H 0.7845 0.4221 0.3211 0.080 Uiso 0.839(7) 1 calc GR . P B 1
C14 C 0.3561(2) 0.47825(15) 0.43991(8) 0.0392(7) Uani 0.673(4) 1 d . . P C 1
H14A H 0.2855 0.4573 0.4292 0.059 Uiso 0.673(4) 1 calc GR . P C 1
H14B H 0.3391 0.5022 0.4651 0.059 Uiso 0.673(4) 1 calc GR . P C 1
H14C H 0.4129 0.4403 0.4443 0.059 Uiso 0.673(4) 1 calc GR . P C 1
C22 C 0.3873(5) 0.72404(16) 0.25840(11) 0.0623(14) Uani 0.699(7) 1 d . . P A 1
H22A H 0.3420 0.7472 0.2375 0.093 Uiso 0.699(7) 1 calc GR . P A 1
H22B H 0.3577 0.6756 0.2630 0.093 Uiso 0.699(7) 1 calc GR . P A 1
H22C H 0.4679 0.7213 0.2501 0.093 Uiso 0.699(7) 1 calc GR . P A 1
C21 C 0.2212(3) 0.7944(3) 0.31462(17) 0.0782(19) Uani 0.699(7) 1 d . . P A 1
H21A H 0.2118 0.8185 0.3403 0.117 Uiso 0.699(7) 1 calc GR . P A 1
H21B H 0.1797 0.7487 0.3150 0.117 Uiso 0.699(7) 1 calc GR . P A 1
H21C H 0.1902 0.8249 0.2935 0.117 Uiso 0.699(7) 1 calc GR . P A 1
C28A C 0.8264(18) 0.3898(10) 0.4132(6) 0.042(4) Uani 0.161(7) 1 d . . P B 2
H28C H 0.8888 0.3565 0.4209 0.050 Uiso 0.161(7) 1 calc R . P B 2
H28D H 0.7624 0.3848 0.4324 0.050 Uiso 0.161(7) 1 calc R . P B 2
C29A C 0.7873(11) 0.3748(6) 0.3731(4) 0.039(4) Uani 0.161(7) 1 d . . P B 2
H29C H 0.7659 0.3235 0.3719 0.047 Uiso 0.161(7) 1 calc R . P B 2
H29D H 0.8533 0.3817 0.3550 0.047 Uiso 0.161(7) 1 calc R . P B 2
C30A C 0.665(2) 0.400(2) 0.3179(11) 0.055(6) Uani 0.161(7) 1 d . . P B 2
H30D H 0.5943 0.4233 0.3089 0.083 Uiso 0.161(7) 1 calc GR . P B 2
H30E H 0.6575 0.3482 0.3157 0.083 Uiso 0.161(7) 1 calc GR . P B 2
H30F H 0.7296 0.4165 0.3014 0.083 Uiso 0.161(7) 1 calc GR . P B 2
C31A C 0.5859(17) 0.3984(8) 0.3791(6) 0.047(4) Uani 0.161(7) 1 d . . P B 2
H31D H 0.5960 0.4123 0.4069 0.071 Uiso 0.161(7) 1 calc GR . P B 2
H31E H 0.5751 0.3464 0.3774 0.071 Uiso 0.161(7) 1 calc GR . P B 2
H31F H 0.5182 0.4227 0.3681 0.071 Uiso 0.161(7) 1 calc GR . P B 2
C22A C 0.3046(12) 0.7299(5) 0.2770(3) 0.071(4) Uani 0.301(7) 1 d . . P A 2
H22D H 0.3653 0.7052 0.2622 0.107 Uiso 0.301(7) 1 calc GR . P A 2
H22E H 0.2604 0.7603 0.2589 0.107 Uiso 0.301(7) 1 calc GR . P A 2
H22F H 0.2536 0.6945 0.2892 0.107 Uiso 0.301(7) 1 calc GR . P A 2
C21A C 0.2465(9) 0.8394(6) 0.3404(4) 0.073(4) Uani 0.301(7) 1 d . U P A 2
H21D H 0.1930 0.8059 0.3530 0.109 Uiso 0.301(7) 1 calc GR . P A 2
H21E H 0.2060 0.8667 0.3198 0.109 Uiso 0.301(7) 1 calc GR . P A 2
H21F H 0.2774 0.8723 0.3603 0.109 Uiso 0.301(7) 1 calc GR . P A 2
Si Si 0.3706(6) 0.7865(4) 0.31650(18) 0.0380(11) Uani 0.301(7) 1 d . . P A 2
N3A N 0.6857(17) 0.4186(11) 0.3568(5) 0.025(4) Uani 0.161(7) 1 d . U P B 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 C15 1.8645(15) . ?
Si1 C18 1.8712(19) . ?
Si1 C16 1.876(2) . ?
Si1 C17 1.866(2) . ?
Si2 C19 1.907(3) . ?
Si2 C20 1.863(3) . ?
Si2 C22 1.877(4) . ?
Si2 C21 1.856(4) . ?
Na1 O1 2.4549(13) . ?
Na1 N1 2.5593(15) . ?
Na1 N3 2.529(3) . ?
Na1 N2 2.6687(15) . ?
Na1 C8 2.9594(15) . ?
Na1 C13 2.9543(17) . ?
Na1 C9 2.9753(16) . ?
Na1 C10 3.0935(17) . ?
Na1 C12 3.0542(19) . ?
Na1 N3A 2.54(2) . ?
O1 C6 1.4014(19) . ?
O1 C7 1.424(2) . ?
N1 C23 1.464(2) . ?
N1 C25 1.474(2) . ?
N1 C24 1.469(2) . ?
N3 C29 1.451(4) . ?
N3 C31 1.469(4) . ?
N3 C30 1.482(8) . ?
N2 C26 1.466(2) . ?
N2 C27 1.458(3) . ?
N2 C28 1.481(4) . ?
N2 C28A 1.523(19) . ?
C1 C6 1.397(2) . ?
C1 C2 1.403(2) . ?
C1 B1 1.654(2) . ?
C8 C13 1.405(2) . ?
C8 C9 1.401(2) . ?
C8 B1 1.645(2) . ?
O2 C13 1.416(2) . ?
O2 C14 1.418(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 H19C 0.9900 . ?
C19 H19D 0.9900 . ?
C19 B1 1.661(2) . ?
C19 Si 1.751(7) . ?
C6 C5 1.393(2) . ?
C13 H13 0.9500 . ?
C13 C12 1.393(2) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 B1 1.665(2) . ?
C5 H5 0.9500 . ?
C5 C4 1.384(3) . ?
C9 H9 0.9500 . ?
C9 C10 1.389(2) . ?
C4 H4 0.9500 . ?
C4 C3 1.377(3) . ?
C2 H2 0.9500 . ?
C2 C3 1.393(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.377(3) . ?
C3 H3 0.9500 . ?
C12 H12 0.9500 . ?
C12 C11 1.396(3) . ?
C11 H11 0.9500 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.508(3) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C20 H20D 0.9800 . ?
C20 H20E 0.9800 . ?
C20 H20F 0.9800 . ?
C20 Si 1.886(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C28 C29 1.517(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C28A H28C 0.9900 . ?
C28A H28D 0.9900 . ?
C28A C29A 1.45(3) . ?
C29A H29C 0.9900 . ?
C29A H29D 0.9900 . ?
C29A N3A 1.54(2) . ?
C30A H30D 0.9800 . ?
C30A H30E 0.9800 . ?
C30A H30F 0.9800 . ?
C30A N3A 1.37(4) . ?
C31A H31D 0.9800 . ?
C31A H31E 0.9800 . ?
C31A H31F 0.9800 . ?
C31A N3A 1.43(2) . ?
C22A H22D 0.9800 . ?
C22A H22E 0.9800 . ?
C22A H22F 0.9800 . ?
C22A Si 1.864(10) . ?
C21A H21D 0.9800 . ?
C21A H21E 0.9800 . ?
C21A H21F 0.9800 . ?
C21A Si 1.924(11) . ?

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
C15 Si1 C18 109.21(8) . . ?
C15 Si1 C16 111.84(8) . . ?
C15 Si1 C17 115.83(8) . . ?
C18 Si1 C16 107.05(12) . . ?
C17 Si1 C18 107.27(11) . . ?
C17 Si1 C16 105.18(12) . . ?
C20 Si2 C19 107.57(15) . . ?
C20 Si2 C22 102.80(17) . . ?
C22 Si2 C19 114.38(16) . . ?
C21 Si2 C19 114.41(18) . . ?
C21 Si2 C20 109.6(2) . . ?
C21 Si2 C22 107.4(3) . . ?
O1 Na1 N1 98.70(5) . . ?
O1 Na1 N3 97.24(9) . . ?
O1 Na1 N2 155.28(5) . . ?
O1 Na1 C8 67.45(4) . . ?
O1 Na1 C13 85.84(4) . . ?
O1 Na1 C9 78.86(5) . . ?
O1 Na1 C10 104.87(5) . . ?
O1 Na1 C12 112.37(5) . . ?
O1 Na1 N3A 95.5(5) . . ?
N1 Na1 N2 71.50(5) . . ?
N1 Na1 C8 123.02(5) . . ?
N1 Na1 C13 143.33(5) . . ?
N1 Na1 C9 97.74(5) . . ?
N1 Na1 C10 89.53(5) . . ?
N1 Na1 C12 129.90(5) . . ?
N3 Na1 N1 122.24(10) . . ?
N3 Na1 N2 71.26(8) . . ?
N3 Na1 C8 114.41(9) . . ?
N3 Na1 C13 92.85(10) . . ?
N3 Na1 C9 139.83(10) . . ?
N3 Na1 C10 137.91(11) . . ?
N3 Na1 C12 92.59(10) . . ?
N2 Na1 C8 137.06(5) . . ?
N2 Na1 C13 115.82(5) . . ?
N2 Na1 C9 124.20(5) . . ?
N2 Na1 C10 97.83(5) . . ?
N2 Na1 C12 90.42(5) . . ?
C8 Na1 C9 27.30(4) . . ?
C8 Na1 C10 47.82(4) . . ?
C8 Na1 C12 48.09(5) . . ?
C13 Na1 C8 27.50(4) . . ?
C13 Na1 C9 47.16(5) . . ?
C13 Na1 C10 54.47(5) . . ?
C13 Na1 C12 26.75(5) . . ?
C9 Na1 C10 26.37(5) . . ?
C9 Na1 C12 54.33(5) . . ?
C12 Na1 C10 45.96(5) . . ?
N3A Na1 N1 114.8(4) . . ?
N3A Na1 N2 69.9(5) . . ?
N3A Na1 C8 121.3(4) . . ?
N3A Na1 C13 100.8(4) . . ?
N3A Na1 C9 147.5(4) . . ?
N3A Na1 C10 145.6(4) . . ?
N3A Na1 C12 100.7(4) . . ?
C6 O1 Na1 120.68(9) . . ?
C6 O1 C7 114.59(13) . . ?
C7 O1 Na1 120.51(11) . . ?
C23 N1 Na1 111.97(11) . . ?
C23 N1 C25 108.01(14) . . ?
C23 N1 C24 108.35(15) . . ?
C25 N1 Na1 104.50(10) . . ?
C24 N1 Na1 113.27(11) . . ?
C24 N1 C25 110.60(14) . . ?
C29 N3 Na1 107.7(2) . . ?
C29 N3 C31 109.4(3) . . ?
C29 N3 C30 111.7(4) . . ?
C31 N3 Na1 114.9(2) . . ?
C31 N3 C30 108.2(3) . . ?
C30 N3 Na1 104.9(4) . . ?
C26 N2 Na1 106.06(11) . . ?
C26 N2 C28 109.2(2) . . ?
C26 N2 C28A 128.9(8) . . ?
C27 N2 Na1 113.84(11) . . ?
C27 N2 C26 109.33(15) . . ?
C27 N2 C28 112.3(2) . . ?
C27 N2 C28A 89.9(8) . . ?
C28 N2 Na1 105.83(16) . . ?
C28A N2 Na1 108.2(8) . . ?
C6 C1 C2 113.71(14) . . ?
C6 C1 B1 123.56(13) . . ?
C2 C1 B1 122.66(13) . . ?
C13 C8 Na1 76.05(9) . . ?
C13 C8 B1 121.09(13) . . ?
C9 C8 Na1 76.98(9) . . ?
C9 C8 C13 115.41(15) . . ?
C9 C8 B1 123.32(14) . . ?
B1 C8 Na1 119.82(9) . . ?
C13 O2 C14 118.12(17) . . ?
Si2 C19 H19A 106.8 . . ?
Si2 C19 H19B 106.8 . . ?
H19A C19 H19B 106.7 . . ?
H19C C19 H19D 106.5 . . ?
B1 C19 Si2 122.05(13) . . ?
B1 C19 H19A 106.8 . . ?
B1 C19 H19B 106.8 . . ?
B1 C19 H19C 106.4 . . ?
B1 C19 H19D 106.4 . . ?
B1 C19 Si 123.7(2) . . ?
Si C19 H19C 106.4 . . ?
Si C19 H19D 106.4 . . ?
C1 C6 O1 117.97(13) . . ?
C5 C6 O1 118.37(14) . . ?
C5 C6 C1 123.63(15) . . ?
Na1 C13 H13 114.3 . . ?
C8 C13 Na1 76.45(9) . . ?
C8 C13 O2 114.93(14) . . ?
C8 C13 H13 118.8 . . ?
O2 C13 Na1 116.28(11) . . ?
C12 C13 Na1 80.63(10) . . ?
C12 C13 C8 122.35(16) . . ?
C12 C13 O2 122.67(16) . . ?
C12 C13 H13 118.8 . . ?
Si1 C15 H15A 106.4 . . ?
Si1 C15 H15B 106.4 . . ?
H15A C15 H15B 106.5 . . ?
B1 C15 Si1 123.65(10) . . ?
B1 C15 H15A 106.4 . . ?
B1 C15 H15B 106.4 . . ?
C6 C5 H5 120.0 . . ?
C4 C5 C6 119.95(15) . . ?
C4 C5 H5 120.0 . . ?
Na1 C9 H9 114.5 . . ?
C8 C9 Na1 75.72(9) . . ?
C8 C9 H9 118.3 . . ?
C10 C9 Na1 81.57(10) . . ?
C10 C9 C8 123.37(17) . . ?
C10 C9 H9 118.3 . . ?
C5 C4 H4 120.5 . . ?
C3 C4 C5 119.02(15) . . ?
C3 C4 H4 120.5 . . ?
C1 C2 H2 118.0 . . ?
C3 C2 C1 124.06(15) . . ?
C3 C2 H2 118.0 . . ?
Na1 C10 H10 119.4 . . ?
C9 C10 Na1 72.06(9) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 Na1 79.15(10) . . ?
C11 C10 C9 119.31(17) . . ?
C11 C10 H10 120.3 . . ?
C4 C3 C2 119.59(16) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
Na1 C12 H12 117.5 . . ?
C13 C12 Na1 72.63(10) . . ?
C13 C12 H12 120.2 . . ?
C13 C12 C11 119.55(17) . . ?
C11 C12 Na1 80.45(11) . . ?
C11 C12 H12 120.2 . . ?
C10 C11 C12 119.95(16) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
N1 C23 H23A 109.5 . . ?
N1 C23 H23B 109.5 . . ?
N1 C23 H23C 109.5 . . ?
H23A C23 H23B 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C25 H25A 108.9 . . ?
N1 C25 H25B 108.9 . . ?
N1 C25 C26 113.46(15) . . ?
H25A C25 H25B 107.7 . . ?
C26 C25 H25A 108.9 . . ?
C26 C25 H25B 108.9 . . ?
N2 C26 C25 112.40(14) . . ?
N2 C26 H26A 109.1 . . ?
N2 C26 H26B 109.1 . . ?
C25 C26 H26A 109.1 . . ?
C25 C26 H26B 109.1 . . ?
H26A C26 H26B 107.9 . . ?
N1 C24 H24A 109.5 . . ?
N1 C24 H24B 109.5 . . ?
N1 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si2 C20 H20A 109.5 . . ?
Si2 C20 H20B 109.5 . . ?
Si2 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
H20D C20 H20E 109.5 . . ?
H20D C20 H20F 109.5 . . ?
H20E C20 H20F 109.5 . . ?
Si C20 H20D 109.5 . . ?
Si C20 H20E 109.5 . . ?
Si C20 H20F 109.5 . . ?
C1 B1 C19 109.11(12) . . ?
C1 B1 C15 110.38(12) . . ?
C8 B1 C1 108.94(12) . . ?
C8 B1 C19 110.87(12) . . ?
C8 B1 C15 106.97(12) . . ?
C19 B1 C15 110.54(12) . . ?
N2 C27 H27A 109.5 . . ?
N2 C27 H27B 109.5 . . ?
N2 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C28 H28A 109.3 . . ?
N2 C28 H28B 109.3 . . ?
N2 C28 C29 111.7(3) . . ?
H28A C28 H28B 107.9 . . ?
C29 C28 H28A 109.3 . . ?
C29 C28 H28B 109.3 . . ?
O1 C7 H7A 109.5 . . ?
O1 C7 H7B 109.5 . . ?
O1 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
Si1 C18 H18A 109.5 . . ?
Si1 C18 H18B 109.5 . . ?
Si1 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Si1 C17 H17A 109.5 . . ?
Si1 C17 H17B 109.5 . . ?
Si1 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N3 C29 C28 113.8(3) . . ?
N3 C29 H29A 108.8 . . ?
N3 C29 H29B 108.8 . . ?
C28 C29 H29A 108.8 . . ?
C28 C29 H29B 108.8 . . ?
H29A C29 H29B 107.7 . . ?
N3 C31 H31A 109.5 . . ?
N3 C31 H31B 109.5 . . ?
N3 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C30 H30A 109.5 . . ?
N3 C30 H30B 109.5 . . ?
N3 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O2 C14 H14A 109.5 . . ?
O2 C14 H14B 109.5 . . ?
O2 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C22 H22A 109.5 . . ?
Si2 C22 H22B 109.5 . . ?
Si2 C22 H22C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si2 C21 H21A 109.5 . . ?
Si2 C21 H21B 109.5 . . ?
Si2 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
N2 C28A H28C 110.6 . . ?
N2 C28A H28D 110.6 . . ?
H28C C28A H28D 108.8 . . ?
C29A C28A N2 105.5(13) . . ?
C29A C28A H28C 110.6 . . ?
C29A C28A H28D 110.6 . . ?
C28A C29A H29C 107.8 . . ?
C28A C29A H29D 107.8 . . ?
C28A C29A N3A 118.1(14) . . ?
H29C C29A H29D 107.1 . . ?
N3A C29A H29C 107.8 . . ?
N3A C29A H29D 107.8 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
N3A C30A H30D 109.5 . . ?
N3A C30A H30E 109.5 . . ?
N3A C30A H30F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
N3A C31A H31D 109.5 . . ?
N3A C31A H31E 109.5 . . ?
N3A C31A H31F 109.5 . . ?
H22D C22A H22E 109.5 . . ?
H22D C22A H22F 109.5 . . ?
H22E C22A H22F 109.5 . . ?
Si C22A H22D 109.5 . . ?
Si C22A H22E 109.5 . . ?
Si C22A H22F 109.5 . . ?
H21D C21A H21E 109.5 . . ?
H21D C21A H21F 109.5 . . ?
H21E C21A H21F 109.5 . . ?
Si C21A H21D 109.5 . . ?
Si C21A H21E 109.5 . . ?
Si C21A H21F 109.5 . . ?
C19 Si C20 113.5(4) . . ?
C19 Si C22A 113.0(4) . . ?
C19 Si C21A 115.6(4) . . ?
C20 Si C21A 98.9(4) . . ?
C22A Si C20 108.5(4) . . ?
C22A Si C21A 106.2(6) . . ?
C29A N3A Na1 108.7(12) . . ?
C30A N3A Na1 122(2) . . ?
C30A N3A C29A 110.0(19) . . ?
C30A N3A C31A 107(2) . . ?
C31A N3A Na1 101.1(11) . . ?
C31A N3A C29A 107.2(15) . . ?

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
Si1 C15 B1 C1 168.17(11) . . . . ?
Si1 C15 B1 C8 49.79(16) . . . . ?
Si1 C15 B1 C19 -71.02(16) . . . . ?
Si2 C19 B1 C1 52.23(18) . . . . ?
Si2 C19 B1 C8 172.21(13) . . . . ?
Si2 C19 B1 C15 -69.34(18) . . . . ?
Na1 O1 C6 C1 77.10(15) . . . . ?
Na1 O1 C6 C5 -101.11(14) . . . . ?
Na1 N1 C25 C26 54.39(16) . . . . ?
Na1 N3 C29 C28 -50.2(3) . . . . ?
Na1 N2 C26 C25 38.08(17) . . . . ?
Na1 N2 C28 C29 -40.3(3) . . . . ?
Na1 N2 C28A C29A 49.4(15) . . . . ?
Na1 C8 C13 O2 -112.97(13) . . . . ?
Na1 C8 C13 C12 69.46(15) . . . . ?
Na1 C8 C9 C10 -69.58(15) . . . . ?
Na1 C8 B1 C1 34.56(14) . . . . ?
Na1 C8 B1 C19 -85.53(13) . . . . ?
Na1 C8 B1 C15 153.88(9) . . . . ?
Na1 C13 C12 C11 67.83(16) . . . . ?
Na1 C9 C10 C11 -65.88(15) . . . . ?
Na1 C10 C11 C12 -60.77(16) . . . . ?
Na1 C12 C11 C10 61.68(16) . . . . ?
O1 C6 C5 C4 176.01(15) . . . . ?
N1 C25 C26 N2 -68.1(2) . . . . ?
N2 C28 C29 N3 65.8(4) . . . . ?
N2 C28A C29A N3A -63.6(19) . . . . ?
C1 C6 C5 C4 -2.1(2) . . . . ?
C1 C2 C3 C4 -0.4(3) . . . . ?
C8 C13 C12 Na1 -67.32(14) . . . . ?
C8 C13 C12 C11 0.5(3) . . . . ?
C8 C9 C10 Na1 66.65(14) . . . . ?
C8 C9 C10 C11 0.8(3) . . . . ?
O2 C13 C12 Na1 115.29(16) . . . . ?
O2 C13 C12 C11 -176.88(16) . . . . ?
C6 C1 C2 C3 -1.4(2) . . . . ?
C6 C1 B1 C8 -59.18(18) . . . . ?
C6 C1 B1 C19 61.99(18) . . . . ?
C6 C1 B1 C15 -176.35(14) . . . . ?
C6 C5 C4 C3 0.1(3) . . . . ?
C13 C8 C9 Na1 67.43(12) . . . . ?
C13 C8 C9 C10 -2.2(2) . . . . ?
C13 C8 B1 C1 -56.66(17) . . . . ?
C13 C8 B1 C19 -176.74(13) . . . . ?
C13 C8 B1 C15 62.66(17) . . . . ?
C13 C12 C11 C10 -2.0(3) . . . . ?
C5 C4 C3 C2 1.1(3) . . . . ?
C9 C8 C13 Na1 -67.97(12) . . . . ?
C9 C8 C13 O2 179.06(14) . . . . ?
C9 C8 C13 C12 1.5(2) . . . . ?
C9 C8 B1 C1 128.34(14) . . . . ?
C9 C8 B1 C19 8.26(19) . . . . ?
C9 C8 B1 C15 -112.34(15) . . . . ?
C9 C10 C11 C12 1.4(3) . . . . ?
C2 C1 C6 O1 -175.48(14) . . . . ?
C2 C1 C6 C5 2.6(2) . . . . ?
C2 C1 B1 C8 124.05(15) . . . . ?
C2 C1 B1 C19 -114.78(16) . . . . ?
C2 C1 B1 C15 6.9(2) . . . . ?
C23 N1 C25 C26 173.76(15) . . . . ?
C26 N2 C28 C29 -154.1(3) . . . . ?
C26 N2 C28A C29A -80.4(15) . . . . ?
C24 N1 C25 C26 -67.83(19) . . . . ?
B1 C1 C6 O1 7.5(2) . . . . ?
B1 C1 C6 C5 -174.41(14) . . . . ?
B1 C1 C2 C3 175.67(16) . . . . ?
B1 C8 C13 Na1 116.66(12) . . . . ?
B1 C8 C13 O2 3.7(2) . . . . ?
B1 C8 C13 C12 -173.89(15) . . . . ?
B1 C8 C9 Na1 -117.31(13) . . . . ?
B1 C8 C9 C10 173.11(14) . . . . ?
B1 C19 Si C20 -172.3(2) . . . . ?
B1 C19 Si C22A -48.2(6) . . . . ?
B1 C19 Si C21A 74.5(5) . . . . ?
C27 N2 C26 C25 -85.07(19) . . . . ?
C27 N2 C28 C29 84.4(3) . . . . ?
C27 N2 C28A C29A 164.5(13) . . . . ?
C28 N2 C26 C25 151.7(2) . . . . ?
C7 O1 C6 C1 -125.87(18) . . . . ?
C7 O1 C6 C5 55.9(2) . . . . ?
C18 Si1 C15 B1 165.01(15) . . . . ?
C16 Si1 C15 B1 -76.69(16) . . . . ?
C17 Si1 C15 B1 43.81(17) . . . . ?
C31 N3 C29 C28 -175.7(3) . . . . ?
C30 N3 C29 C28 64.5(5) . . . . ?
C14 O2 C13 Na1 116.16(19) . . . . ?
C14 O2 C13 C8 -157.20(19) . . . . ?
C14 O2 C13 C12 20.4(3) . . . . ?
C28A N2 C26 C25 168.6(10) . . . . ?
C28A C29A N3A Na1 40.9(17) . . . . ?
C28A C29A N3A C30A 176(2) . . . . ?
C28A C29A N3A C31A -68(2) . . . . ?
Si C19 B1 C1 66.5(3) . . . . ?
Si C19 B1 C8 -173.6(3) . . . . ?
Si C19 B1 C15 -55.1(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
        Empirical correction (ABSPACK) includes:
        - Absorption correction using spherical harmonics
        - Frame scaling
;
