#------------------------------------------------------------------------------
#$Date: 2023-07-05 12:34:36 +0300 (Wed, 05 Jul 2023) $
#$Revision: 284883 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/90/1569051.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1569051
loop_
_publ_author_name
'Tortajada, Andreu'
'Bole, Leonie J.'
'Mu, Manting'
'Stanford, Martin'
'Peñas-Defrutos, Marconi N'
'García-Melchor, Max'
'Hevia, Eva'
_publ_section_title
;
 Sodium mediated deprotonative borylation of arenes using sterically
 demanding B(CH₂SiMe₃)₃: unlocking
 polybasic behaviour and competing lateral borane sodiation.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6538
_journal_page_last               6545
_journal_paper_doi               10.1039/d3sc01705b
_journal_volume                  14
_journal_year                    2023
_chemical_formula_moiety         'C29 H55 B N3 Na Si2'
_chemical_formula_sum            'C29 H55 B N3 Na Si2'
_chemical_formula_weight         535.74
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-07-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-03-01 deposited with the CCDC.	2023-05-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.3580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.08170(10)
_cell_length_b                   18.6842(2)
_cell_length_c                   16.2208(2)
_cell_measurement_reflns_used    15566
_cell_measurement_temperature    100.3(5)
_cell_measurement_theta_max      76.6680
_cell_measurement_theta_min      3.6010
_cell_volume                     3352.79(6)
_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)'
_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_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.061
_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
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.553
_refine_diff_density_rms         0.063
_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_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0643
_refine_ls_R_factor_gt           0.0549
_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
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5830
_reflns_number_total             6931
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc01705b2.cif
_cod_data_source_block           20EH146_MWS155
_cod_depositor_comments
'Adding full bibliography for 1569049--1569054.cif.'
_cod_database_code               1569051
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C120 H212 B4 N8 Na4 Si8 '
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.828
_diffrn_oxdiff_digest_frames
;
01feacc35055c5b62f8c66d86d515f362a000371bc6
;
_diffrn_oxdiff_digest_hkl
;
0106a8c953b5e480a0a300a22f85f604ea4486
;
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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)
;
_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
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'
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
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'
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_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_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) . . . . ?
