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

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

data_TS1P
_database_code_depnum_ccdc_archive 'CCDC 2102894'
loop_
_audit_author_name
_audit_author_address
'Vladimir Chernyshev'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2021-08-12 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;

_audit_creation_method           'MRIA, SHELXL-97'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 N O48 Si24'
_chemical_formula_weight         1600.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   20.0526(11)
_cell_length_b                   19.9323(11)
_cell_length_c                   13.4069(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5358.7(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4070
_cell_measurement_theta_min      0.915
_cell_measurement_theta_max      11.499

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3196
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              15 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              0.7 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              0.7 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 
Specimen was sealed in a 0.7 mm diameter borosilicate glass capillary
;
_pd_spec_mount_mode              transmission # options are 'reflection' 
# or 'transmission'

_pd_spec_shape                   cylinder # options are 'cylinder',
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     'no specific habit'
_pd_char_colour                  'light grey' # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen. 
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.



_pd_prep_cool_rate               ?
_pd_prep_pressure                101
_pd_prep_temperature             295(2)




# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
ID22 beam line, ESRF, Grenoble, France
;

_diffrn_ambient_temperature      295(2)
_diffrn_source                   'ID22 bending magnet at ESRF'
_diffrn_source_target            ?
_diffrn_source_type              'synchrotron radiation'
_diffrn_measurement_device_type  'ESRF powder diffractometer'
_diffrn_detector                 ?
_diffrn_detector_type            'scintillation counter'
_pd_meas_scan_method             cont # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         ?

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.354345(4)
_diffrn_radiation_monochromator  'Si 111 double crystal'

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        11001
_pd_meas_2theta_range_min        1.000
_pd_meas_2theta_range_max        23.000
_pd_meas_2theta_range_inc        0.002

# The following fields are used to identify the programs used.

_computing_data_collection       'local program'
_computing_cell_refinement       'LSPAID (Visser et al., 1986)'
_computing_data_reduction        'MRIA (Zlokazov et al., 1992)'
_computing_structure_solution    MRIA
_computing_structure_refinement  MRIA
_computing_molecular_graphics    Mercury
_computing_publication_material  'SHELXL-97 and MRIA'


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
Anisotropic line broadening has been taken into account (Popa, 1998)
;

# The next three items are given as text
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     ?

_pd_proc_ls_prof_R_factor        0.0430
_pd_proc_ls_prof_wR_factor       0.0557
_pd_proc_ls_prof_wR_expected     0.0169

_refine_special_details          
; 
?
;

_refine_ls_R_I_factor            0.1093
_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     157
_refine_ls_number_restraints     92
_refine_ls_number_constraints    37
# The following item is the same as CHI, the square root of 'CHI squared = 9.349'
_refine_ls_goodness_of_fit_all   3.058

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
_pd_proc_2theta_range_min        1.000
_pd_proc_2theta_range_max        23.000
_pd_proc_2theta_range_inc        0.002

_pd_proc_wavelength              0.354345(4)

_pd_block_diffractogram_id       TS1P_pattern # The id used for the block
#                                              # containing the powder 
#                                             # pattern profile (section 11).

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.42279(18) 0.05810(16) -0.3358(3) 0.0191(5) Uiso 1 1 d . . .
Si2 Si 0.30510(17) 0.02800(17) -0.1880(3) 0.0191(5) Uiso 1 1 d . . .
Si3 Si 0.27631(18) 0.05611(18) 0.0310(3) 0.0191(5) Uiso 1 1 d . . .
Si4 Si 0.11781(18) 0.06250(16) 0.0288(3) 0.0191(5) Uiso 1 1 d . . .
Si5 Si 0.07120(18) 0.02759(17) -0.1855(2) 0.0191(5) Uiso 1 1 d . . .
Si6 Si 0.18790(18) 0.06009(16) -0.3257(3) 0.0191(5) Uiso 1 1 d . . .
Si7 Si 0.42510(18) -0.17120(18) -0.3287(2) 0.0191(5) Uiso 1 1 d . . .
Si8 Si 0.30670(18) -0.13161(17) -0.1866(3) 0.0191(5) Uiso 1 1 d . . .
Si9 Si 0.27710(18) -0.1750(2) 0.0307(2) 0.0191(5) Uiso 1 1 d . . .
Si10 Si 0.12440(17) -0.1740(2) 0.0321(2) 0.0191(5) Uiso 1 1 d . . .
Si11 Si 0.07290(19) -0.13020(17) -0.1789(2) 0.0191(5) Uiso 1 1 d . . .
Si12 Si 0.18540(17) -0.17350(17) -0.3217(2) 0.0191(5) Uiso 1 1 d . . .
O1 O 0.3750(4) 0.0459(3) -0.2407(6) 0.0202(7) Uiso 1 1 d . . .
O2 O 0.3059(4) 0.0618(3) -0.0800(6) 0.0202(7) Uiso 1 1 d . . .
O3 O 0.1974(4) 0.0603(4) 0.0249(6) 0.0202(7) Uiso 1 1 d . . .
O4 O 0.0954(4) 0.0639(3) -0.0848(6) 0.0202(7) Uiso 1 1 d . . .
O5 O 0.1151(4) 0.0599(3) -0.2742(6) 0.0202(7) Uiso 1 1 d . . .
O6 O 0.2474(4) 0.0671(4) -0.2482(6) 0.0202(7) Uiso 1 1 d . . .
O7 O 0.3744(4) -0.1563(4) -0.2390(6) 0.0202(7) Uiso 1 1 d . . .
O8 O 0.3106(4) -0.1523(4) -0.0716(6) 0.0202(7) Uiso 1 1 d . . .
O9 O 0.2009(4) -0.1513(4) 0.0260(5) 0.0202(7) Uiso 1 1 d . . .
O10 O 0.0923(4) -0.1650(4) -0.0754(5) 0.0202(7) Uiso 1 1 d . . .
O11 O 0.1158(4) -0.1531(3) -0.2733(6) 0.0202(7) Uiso 1 1 d . . .
O12 O 0.2434(3) -0.1595(4) -0.2440(5) 0.0202(7) Uiso 1 1 d . . .
O13 O 0.3059(4) -0.0517(3) -0.1927(6) 0.0202(7) Uiso 1 1 d . . .
O14 O 0.0790(4) -0.0509(3) -0.1674(5) 0.0202(7) Uiso 1 1 d . . .
O15 O 0.4155(4) 0.1300(4) -0.3879(5) 0.0202(7) Uiso 1 1 d . . .
O16 O 0.4047(4) -0.0008(4) -0.4117(5) 0.0202(7) Uiso 1 1 d . . .
O17 O 0.4043(4) -0.1352(4) -0.4315(6) 0.0202(7) Uiso 1 1 d . . .
O18 O 0.1855(4) 0.1303(4) -0.3860(6) 0.0202(7) Uiso 1 1 d . . .
O19 O 0.1906(4) 0.0008(4) -0.4040(6) 0.0202(7) Uiso 1 1 d . . .
O20 O 0.1983(4) -0.1316(4) -0.4218(6) 0.0202(7) Uiso 1 1 d . . .
O21 O -0.0047(4) 0.0457(4) -0.2085(6) 0.0202(7) Uiso 1 1 d . . .
O22 O -0.0001(3) -0.1577(4) -0.2057(6) 0.0202(7) Uiso 1 1 d . . .
O23 O 0.4227(6) -0.2500 -0.3556(7) 0.0202(7) Uiso 1 2 d S . .
O24 O 0.1984(5) -0.2500 -0.3516(8) 0.0202(7) Uiso 1 2 d S . .
O25 O 0.2950(5) -0.2500 0.0655(8) 0.0202(7) Uiso 1 2 d S . .
O26 O 0.1167(5) -0.2500 0.0687(8) 0.0202(7) Uiso 1 2 d S . .
N1 N 0.4762 0.2500 -0.1090 0.101 Uiso 1 2 d S . .
C1 C 0.4950 0.2330 -0.2210 0.101 Uiso 0.30 1 d P . .
C2 C 0.5680 0.2500 -0.2410 0.101 Uiso 0.60 2 d SP . .
C3 C 0.5780 0.2500 -0.3620 0.101 Uiso 0.60 2 d SP . .
C4 C 0.3990 0.2740 -0.1000 0.101 Uiso 0.30 1 d P . .
C5 C 0.3550 0.2280 -0.1500 0.101 Uiso 0.30 1 d P . .
C6 C 0.2780 0.2500 -0.1470 0.101 Uiso 0.60 2 d SP . .
C7 C 0.4960 0.4120 0.0450 0.101 Uiso 0.30 1 d P . .
C8 C 0.4730 0.3340 -0.0190 0.101 Uiso 0.30 1 d P . .
C9 C 0.4960 0.4120 0.0450 0.101 Uiso 0.50 1 d P . .
C10 C 0.5080 0.1990 -0.0320 0.101 Uiso 0.50 1 d P . .
C11 C 0.4900 0.1240 -0.0450 0.101 Uiso 0.50 1 d P . .
C12 C 0.5290 0.0880 0.0330 0.101 Uiso 0.50 1 d P . .
C21 C 0.4130 0.2290 -0.1660 0.101 Uiso 0.20 1 d P . .
C22 C 0.3550 0.2720 -0.1500 0.101 Uiso 0.20 1 d P . .
C23 C 0.2850 0.2500 -0.1950 0.101 Uiso 0.40 2 d SP . .
C24 C 0.5340 0.2790 -0.1850 0.101 Uiso 0.20 1 d P . .
C25 C 0.5460 0.2250 -0.2630 0.101 Uiso 0.20 1 d P . .
C26 C 0.6010 0.2500 -0.3320 0.101 Uiso 0.40 2 d SP . .
C27 C 0.4680 0.3150 -0.0600 0.101 Uiso 0.20 1 d P . .
C28 C 0.5160 0.3350 0.0200 0.101 Uiso 0.20 1 d P . .

_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 O21 1.590(8) 6_655 ?
Si1 O16 1.595(8) . ?
Si1 O15 1.601(8) . ?
Si1 O1 1.613(8) . ?
Si2 O13 1.590(8) . ?
Si2 O2 1.597(9) . ?
Si2 O1 1.610(8) . ?
Si2 O6 1.612(9) . ?
Si3 O19 1.577(8) 2 ?
Si3 O3 1.587(9) . ?
Si3 O2 1.606(9) . ?
Si3 O20 1.709(8) 2 ?
Si4 O16 1.534(8) 2 ?
Si4 O4 1.588(9) . ?
Si4 O3 1.597(9) . ?
Si4 O17 1.606(8) 2 ?
Si5 O14 1.591(8) . ?
Si5 O21 1.594(8) . ?
Si5 O4 1.607(9) . ?
Si5 O5 1.614(8) . ?
Si6 O19 1.581(8) . ?
Si6 O6 1.588(9) . ?
Si6 O5 1.615(9) . ?
Si6 O18 1.617(8) . ?
Si7 O22 1.592(8) 6_655 ?
Si7 O7 1.602(8) . ?
Si7 O17 1.609(8) . ?
Si7 O23 1.612(4) . ?
Si8 O12 1.585(8) . ?
Si8 O13 1.595(8) . ?
Si8 O8 1.598(8) . ?
Si8 O7 1.606(8) . ?
Si9 O8 1.593(8) . ?
Si9 O9 1.600(9) . ?
Si9 O25 1.607(5) . ?
Si9 O18 1.613(8) 2 ?
Si10 O10 1.589(8) . ?
Si10 O26 1.600(5) . ?
Si10 O15 1.600(8) 2 ?
Si10 O9 1.602(9) . ?
Si11 O14 1.593(8) . ?
Si11 O11 1.597(8) . ?
Si11 O10 1.599(8) . ?
Si11 O22 1.604(8) . ?
Si12 O12 1.586(8) . ?
Si12 O11 1.592(8) . ?
Si12 O24 1.598(5) . ?
Si12 O20 1.602(8) . ?
O15 Si10 1.600(8) 2_554 ?
O16 Si4 1.534(8) 2_554 ?
O17 Si4 1.606(8) 2_554 ?
O18 Si9 1.613(8) 2_554 ?
O19 Si3 1.577(8) 2_554 ?
O20 Si3 1.709(8) 2_554 ?
O21 Si1 1.590(8) 6 ?
O22 Si7 1.592(8) 6 ?
O23 Si7 1.612(4) 8 ?
O24 Si12 1.598(5) 8 ?
O25 Si9 1.607(5) 8 ?
O26 Si10 1.600(5) 8 ?

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
O21 Si1 O16 109.4(4) 6_655 . ?
O21 Si1 O15 112.7(4) 6_655 . ?
O16 Si1 O15 111.1(4) . . ?
O21 Si1 O1 103.0(4) 6_655 . ?
O16 Si1 O1 104.9(4) . . ?
O15 Si1 O1 115.2(4) . . ?
O13 Si2 O2 117.2(4) . . ?
O13 Si2 O1 101.3(4) . . ?
O2 Si2 O1 107.2(4) . . ?
O13 Si2 O6 118.1(4) . . ?
O2 Si2 O6 104.9(4) . . ?
O1 Si2 O6 107.3(4) . . ?
O19 Si3 O3 119.1(5) 2 . ?
O19 Si3 O2 114.0(4) 2 . ?
O3 Si3 O2 108.5(5) . . ?
O19 Si3 O20 107.6(4) 2 2 ?
O3 Si3 O20 105.7(4) . 2 ?
O2 Si3 O20 99.8(4) . 2 ?
O16 Si4 O4 115.4(4) 2 . ?
O16 Si4 O3 106.8(5) 2 . ?
O4 Si4 O3 104.6(5) . . ?
O16 Si4 O17 118.0(5) 2 2 ?
O4 Si4 O17 103.0(4) . 2 ?
O3 Si4 O17 108.1(4) . 2 ?
O14 Si5 O21 110.3(4) . . ?
O14 Si5 O4 106.6(4) . . ?
O21 Si5 O4 110.4(4) . . ?
O14 Si5 O5 116.8(4) . . ?
O21 Si5 O5 106.7(4) . . ?
O4 Si5 O5 105.9(4) . . ?
O19 Si6 O6 118.3(4) . . ?
O19 Si6 O5 108.2(4) . . ?
O6 Si6 O5 113.5(5) . . ?
O19 Si6 O18 108.4(4) . . ?
O6 Si6 O18 105.9(4) . . ?
O5 Si6 O18 100.9(4) . . ?
O22 Si7 O7 110.4(4) 6_655 . ?
O22 Si7 O17 114.7(4) 6_655 . ?
O7 Si7 O17 113.3(4) . . ?
O22 Si7 O23 104.9(5) 6_655 . ?
O7 Si7 O23 109.2(5) . . ?
O17 Si7 O23 103.6(5) . . ?
O12 Si8 O13 108.5(4) . . ?
O12 Si8 O8 114.7(4) . . ?
O13 Si8 O8 107.9(4) . . ?
O12 Si8 O7 110.9(4) . . ?
O13 Si8 O7 107.0(4) . . ?
O8 Si8 O7 107.6(4) . . ?
O8 Si9 O9 106.6(4) . . ?
O8 Si9 O25 114.8(5) . . ?
O9 Si9 O25 120.0(5) . . ?
O8 Si9 O18 104.1(4) . 2 ?
O9 Si9 O18 107.9(4) . 2 ?
O25 Si9 O18 102.1(5) . 2 ?
O10 Si10 O26 110.3(5) . . ?
O10 Si10 O15 110.1(4) . 2 ?
O26 Si10 O15 105.4(5) . 2 ?
O10 Si10 O9 108.1(4) . . ?
O26 Si10 O9 112.1(5) . . ?
O15 Si10 O9 111.0(4) 2 . ?
O14 Si11 O11 108.6(4) . . ?
O14 Si11 O10 109.1(4) . . ?
O11 Si11 O10 115.6(4) . . ?
O14 Si11 O22 115.5(4) . . ?
O11 Si11 O22 102.5(4) . . ?
O10 Si11 O22 105.6(4) . . ?
O12 Si12 O11 109.3(4) . . ?
O12 Si12 O24 102.3(5) . . ?
O11 Si12 O24 119.3(5) . . ?
O12 Si12 O20 109.9(4) . . ?
O11 Si12 O20 110.5(4) . . ?
O24 Si12 O20 105.2(5) . . ?
Si2 O1 Si1 153.8(6) . . ?
Si2 O2 Si3 143.8(5) . . ?
Si3 O3 Si4 175.0(6) . . ?
Si4 O4 Si5 152.0(5) . . ?
Si5 O5 Si6 144.0(5) . . ?
Si6 O6 Si2 145.5(5) . . ?
Si7 O7 Si8 157.2(5) . . ?
Si9 O8 Si8 152.1(6) . . ?
Si9 O9 Si10 146.0(6) . . ?
Si10 O10 Si11 159.2(6) . . ?
Si12 O11 Si11 150.3(5) . . ?
Si8 O12 Si12 165.4(5) . . ?
Si2 O13 Si8 174.8(6) . . ?
Si5 O14 Si11 162.5(6) . . ?
Si10 O15 Si1 146.0(6) 2_554 . ?
Si4 O16 Si1 171.4(6) 2_554 . ?
Si4 O17 Si7 139.3(5) 2_554 . ?
Si9 O18 Si6 144.1(6) 2_554 . ?
Si3 O19 Si6 156.8(6) 2_554 . ?
Si12 O20 Si3 144.8(5) . 2_554 ?
Si1 O21 Si5 146.7(6) 6 . ?
Si7 O22 Si11 148.5(6) 6 . ?
Si7 O23 Si7 153.9(7) 8 . ?
Si12 O24 Si12 145.2(8) 8 . ?
Si9 O25 Si9 137.0(7) 8 . ?
Si10 O26 Si10 142.5(8) 8 . ?

_refine_diff_density_max         0.74
_refine_diff_density_min         -0.53
_refine_diff_density_rms         0.33
####################################################################### 
# 
# 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_TS1P75
_database_code_depnum_ccdc_archive 'CCDC 2102895'
loop_
_audit_author_name
_audit_author_address
'Vladimir Chernyshev'
;Lomonosov Moscow State University
Russia
;
_audit_update_record             
;
2021-08-12 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;

_audit_creation_method           'MRIA, SHELXL-97'
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 N O48 Si24'
_chemical_formula_weight         1600.29

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0522 0.0431 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0030 0.0019 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0015 0.0009 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   Pnma
_symmetry_space_group_name_Hall  '-P 2ac 2n'

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

_cell_length_a                   20.0518(12)
_cell_length_b                   19.9318(11)
_cell_length_c                   13.4065(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5358.2(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    4070
_cell_measurement_theta_min      0.916
_cell_measurement_theta_max      11.500

_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3196
_exptl_absorpt_coefficient_mu    0.352
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.
_pd_spec_size_axial              15 # perpendicular to 
# equatorial plane

_pd_spec_size_equat              0.7 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              0.7 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
; 
Specimen was sealed in a 0.7 mm diameter borosilicate glass capillary
;
_pd_spec_mount_mode              transmission # options are 'reflection' 
# or 'transmission'

_pd_spec_shape                   cylinder # options are 'cylinder',
# 'flat_sheet' or 'irregular'

_pd_char_particle_morphology     'no specific habit'
_pd_char_colour                  'light grey' # use ICDD colour descriptions

# The following three fields describe the preparation of the specimen. 
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.



_pd_prep_cool_rate               ?
_pd_prep_pressure                101
_pd_prep_temperature             295(2)




# 7. EXPERIMENTAL DATA

_exptl_special_details           
; ?
;

# This following item is used to identify the equipment used to record the
# powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; 
ID22 beam line, ESRF, Grenoble, France
;

_diffrn_ambient_temperature      295(2)
_diffrn_source                   'ID22 bending magnet at ESRF'
_diffrn_source_target            ?
_diffrn_source_type              'synchrotron radiation'
_diffrn_measurement_device_type  'ESRF powder diffractometer'
_diffrn_detector                 ?
_diffrn_detector_type            'scintillation counter'
_pd_meas_scan_method             cont # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         ?

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.354345(4)
_diffrn_radiation_monochromator  'Si 111 double crystal'

# The following four items give details of the measured (not processed)
# powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        11001
_pd_meas_2theta_range_min        1.000
_pd_meas_2theta_range_max        23.000
_pd_meas_2theta_range_inc        0.002

# The following fields are used to identify the programs used.

_computing_data_collection       'local program'
_computing_cell_refinement       'LSPAID (Visser et al., 1986)'
_computing_data_reduction        'MRIA (Zlokazov et al., 1992)'
_computing_structure_solution    MRIA
_computing_structure_refinement  MRIA
_computing_molecular_graphics    Mercury
_computing_publication_material  'SHELXL-97 and MRIA'


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
Anisotropic line broadening has been taken into account (Popa, 1998)
;

# The next three items are given as text
_pd_proc_ls_profile_function     'split-type pseudo-Voigt (Toraya, 1986)'
_pd_proc_ls_background_function  'Chebyshev polynomial up to the 5th order'
_pd_proc_ls_pref_orient_corr     ?

_pd_proc_ls_prof_R_factor        0.0418
_pd_proc_ls_prof_wR_factor       0.0543
_pd_proc_ls_prof_wR_expected     0.0191

_refine_special_details          
; 
?
;

_refine_ls_R_I_factor            0.1102
_refine_ls_structure_factor_coef Inet
_refine_ls_matrix_type           fullcycle
_refine_ls_weighting_scheme      sigma
_refine_ls_hydrogen_treatment    noref
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     157
_refine_ls_number_restraints     92
_refine_ls_number_constraints    37
# The following item is the same as CHI, the square root of 'CHI squared = 6.938'
_refine_ls_goodness_of_fit_all   2.634

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.002


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.
_pd_proc_2theta_range_min        1.000
_pd_proc_2theta_range_max        23.000
_pd_proc_2theta_range_inc        0.002

_pd_proc_wavelength              0.354345(4)

_pd_block_diffractogram_id       TS1P75_pattern # The id used for the block
#                                              # containing the powder 
#                                             # pattern profile (section 11).

# Give appropriate details in the next two text fields.
_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

#==============================================================================

# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.42269(18) 0.05800(16) -0.3356(3) 0.0189(5) Uiso 1 1 d . . .
Si2 Si 0.30500(17) 0.02810(17) -0.1883(3) 0.0189(5) Uiso 1 1 d . . .
Si3 Si 0.27661(19) 0.05621(18) 0.0312(3) 0.0189(5) Uiso 1 1 d . . .
Si4 Si 0.11791(18) 0.06190(17) 0.0291(3) 0.0189(5) Uiso 1 1 d . . .
Si5 Si 0.07130(18) 0.02759(17) -0.1852(2) 0.0189(5) Uiso 1 1 d . . .
Si6 Si 0.18770(18) 0.06059(16) -0.3255(3) 0.0189(5) Uiso 1 1 d . . .
Si7 Si 0.42490(18) -0.17130(18) -0.3288(2) 0.0189(5) Uiso 1 1 d . . .
Si8 Si 0.30680(18) -0.13161(17) -0.1863(3) 0.0189(5) Uiso 1 1 d . . .
Si9 Si 0.27700(18) -0.1750(2) 0.0309(2) 0.0189(5) Uiso 1 1 d . . .
Si10 Si 0.12440(17) -0.1739(2) 0.0322(2) 0.0189(5) Uiso 1 1 d . . .
Si11 Si 0.07280(19) -0.13020(17) -0.1792(2) 0.0189(5) Uiso 1 1 d . . .
Si12 Si 0.18550(17) -0.17340(18) -0.3221(2) 0.0189(5) Uiso 1 1 d . . .
O1 O 0.3751(4) 0.0455(3) -0.2406(6) 0.0211(8) Uiso 1 1 d . . .
O2 O 0.3062(4) 0.0619(3) -0.0801(6) 0.0211(8) Uiso 1 1 d . . .
O3 O 0.1975(4) 0.0600(4) 0.0243(6) 0.0211(8) Uiso 1 1 d . . .
O4 O 0.0952(4) 0.0641(3) -0.0846(6) 0.0211(8) Uiso 1 1 d . . .
O5 O 0.1151(4) 0.0597(3) -0.2739(6) 0.0211(8) Uiso 1 1 d . . .
O6 O 0.2475(4) 0.0674(4) -0.2483(6) 0.0211(8) Uiso 1 1 d . . .
O7 O 0.3744(4) -0.1561(4) -0.2389(6) 0.0211(8) Uiso 1 1 d . . .
O8 O 0.3108(4) -0.1519(4) -0.0713(6) 0.0211(8) Uiso 1 1 d . . .
O9 O 0.2009(4) -0.1510(4) 0.0254(5) 0.0211(8) Uiso 1 1 d . . .
O10 O 0.0926(4) -0.1657(4) -0.0763(5) 0.0211(8) Uiso 1 1 d . . .
O11 O 0.1157(4) -0.1524(3) -0.2741(6) 0.0211(8) Uiso 1 1 d . . .
O12 O 0.2433(3) -0.1597(4) -0.2436(5) 0.0211(8) Uiso 1 1 d . . .
O13 O 0.3057(4) -0.0516(4) -0.1929(6) 0.0211(8) Uiso 1 1 d . . .
O14 O 0.0787(4) -0.0509(3) -0.1666(5) 0.0211(8) Uiso 1 1 d . . .
O15 O 0.4150(4) 0.1299(4) -0.3877(5) 0.0211(8) Uiso 1 1 d . . .
O16 O 0.4052(4) -0.0011(4) -0.4116(5) 0.0211(8) Uiso 1 1 d . . .
O17 O 0.4042(4) -0.1356(4) -0.4316(6) 0.0211(8) Uiso 1 1 d . . .
O18 O 0.1849(4) 0.1308(4) -0.3850(6) 0.0211(8) Uiso 1 1 d . . .
O19 O 0.1906(4) 0.0013(4) -0.4043(6) 0.0211(8) Uiso 1 1 d . . .
O20 O 0.1991(4) -0.1313(4) -0.4217(6) 0.0211(8) Uiso 1 1 d . . .
O21 O -0.0047(4) 0.0456(4) -0.2087(6) 0.0211(8) Uiso 1 1 d . . .
O22 O -0.0001(3) -0.1579(4) -0.2058(6) 0.0211(8) Uiso 1 1 d . . .
O23 O 0.4230(6) -0.2500 -0.3550(8) 0.0211(8) Uiso 1 2 d S . .
O24 O 0.1980(5) -0.2500 -0.3516(8) 0.0211(8) Uiso 1 2 d S . .
O25 O 0.2947(6) -0.2500 0.0656(8) 0.0211(8) Uiso 1 2 d S . .
O26 O 0.1172(5) -0.2500 0.0690(8) 0.0211(8) Uiso 1 2 d S . .
N1 N 0.4762 0.2500 -0.1090 0.101 Uiso 1 2 d S . .
C1 C 0.4950 0.2330 -0.2210 0.101 Uiso 0.30 1 d P . .
C2 C 0.5680 0.2500 -0.2410 0.101 Uiso 0.60 2 d SP . .
C3 C 0.5780 0.2500 -0.3620 0.101 Uiso 0.60 2 d SP . .
C4 C 0.3990 0.2740 -0.1000 0.101 Uiso 0.30 1 d P . .
C5 C 0.3550 0.2280 -0.1500 0.101 Uiso 0.30 1 d P . .
C6 C 0.2780 0.2500 -0.1470 0.101 Uiso 0.60 2 d SP . .
C7 C 0.4960 0.4120 0.0450 0.101 Uiso 0.30 1 d P . .
C8 C 0.4730 0.3340 -0.0190 0.101 Uiso 0.30 1 d P . .
C9 C 0.4960 0.4120 0.0450 0.101 Uiso 0.50 1 d P . .
C10 C 0.5080 0.1990 -0.0320 0.101 Uiso 0.50 1 d P . .
C11 C 0.4900 0.1240 -0.0450 0.101 Uiso 0.50 1 d P . .
C12 C 0.5290 0.0880 0.0330 0.101 Uiso 0.50 1 d P . .
C21 C 0.4130 0.2290 -0.1660 0.101 Uiso 0.20 1 d P . .
C22 C 0.3550 0.2720 -0.1500 0.101 Uiso 0.20 1 d P . .
C23 C 0.2850 0.2500 -0.1950 0.101 Uiso 0.40 2 d SP . .
C24 C 0.5340 0.2790 -0.1850 0.101 Uiso 0.20 1 d P . .
C25 C 0.5460 0.2250 -0.2630 0.101 Uiso 0.20 1 d P . .
C26 C 0.6010 0.2500 -0.3320 0.101 Uiso 0.40 2 d SP . .
C27 C 0.4680 0.3150 -0.0600 0.101 Uiso 0.20 1 d P . .
C28 C 0.5160 0.3350 0.0200 0.101 Uiso 0.20 1 d P . .

_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 O21 1.592(9) 6_655 ?
Si1 O16 1.596(8) . ?
Si1 O15 1.601(8) . ?
Si1 O1 1.611(9) . ?
Si2 O13 1.590(8) . ?
Si2 O2 1.600(9) . ?
Si2 O1 1.609(9) . ?
Si2 O6 1.609(9) . ?
Si3 O19 1.580(8) 2 ?
Si3 O3 1.591(9) . ?
Si3 O2 1.610(9) . ?
Si3 O20 1.695(8) 2 ?
Si4 O16 1.522(8) 2 ?
Si4 O4 1.592(9) . ?
Si4 O3 1.598(9) . ?
Si4 O17 1.622(8) 2 ?
Si5 O14 1.591(8) . ?
Si5 O21 1.597(9) . ?
Si5 O4 1.606(9) . ?
Si5 O5 1.611(9) . ?
Si6 O19 1.586(8) . ?
Si6 O6 1.590(9) . ?
Si6 O18 1.612(8) . ?
Si6 O5 1.612(9) . ?
Si7 O22 1.596(8) 6_655 ?
Si7 O7 1.603(8) . ?
Si7 O17 1.606(8) . ?
Si7 O23 1.608(4) . ?
Si8 O12 1.589(8) . ?
Si8 O8 1.596(8) . ?
Si8 O13 1.598(8) . ?
Si8 O7 1.604(8) . ?
Si9 O8 1.596(8) . ?
Si9 O9 1.601(9) . ?
Si9 O25 1.605(5) . ?
Si9 O18 1.622(8) 2 ?
Si10 O15 1.596(8) 2 ?
Si10 O10 1.596(8) . ?
Si10 O26 1.602(5) . ?
Si10 O9 1.603(9) . ?
Si11 O14 1.594(8) . ?
Si11 O11 1.598(8) . ?
Si11 O10 1.600(8) . ?
Si11 O22 1.603(8) . ?
Si12 O12 1.589(8) . ?
Si12 O11 1.596(8) . ?
Si12 O24 1.597(5) . ?
Si12 O20 1.601(8) . ?
O15 Si10 1.596(8) 2_554 ?
O16 Si4 1.522(8) 2_554 ?
O17 Si4 1.622(8) 2_554 ?
O18 Si9 1.622(8) 2_554 ?
O19 Si3 1.580(8) 2_554 ?
O20 Si3 1.695(8) 2_554 ?
O21 Si1 1.592(9) 6 ?
O22 Si7 1.596(8) 6 ?
O23 Si7 1.608(4) 8 ?
O24 Si12 1.597(5) 8 ?
O25 Si9 1.605(5) 8 ?
O26 Si10 1.602(5) 8 ?

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
O21 Si1 O16 108.9(4) 6_655 . ?
O21 Si1 O15 112.9(5) 6_655 . ?
O16 Si1 O15 111.2(4) . . ?
O21 Si1 O1 102.9(4) 6_655 . ?
O16 Si1 O1 105.1(4) . . ?
O15 Si1 O1 115.2(4) . . ?
O13 Si2 O2 117.1(4) . . ?
O13 Si2 O1 101.0(4) . . ?
O2 Si2 O1 106.9(4) . . ?
O13 Si2 O6 118.3(4) . . ?
O2 Si2 O6 105.0(4) . . ?
O1 Si2 O6 107.6(4) . . ?
O19 Si3 O3 118.8(5) 2 . ?
O19 Si3 O2 113.9(4) 2 . ?
O3 Si3 O2 108.1(5) . . ?
O19 Si3 O20 108.5(4) 2 2 ?
O3 Si3 O20 105.5(4) . 2 ?
O2 Si3 O20 100.2(4) . 2 ?
O16 Si4 O4 115.8(4) 2 . ?
O16 Si4 O3 107.8(5) 2 . ?
O4 Si4 O3 104.3(5) . . ?
O16 Si4 O17 117.9(5) 2 2 ?
O4 Si4 O17 102.0(4) . 2 ?
O3 Si4 O17 107.9(5) . 2 ?
O14 Si5 O21 109.9(4) . . ?
O14 Si5 O4 106.6(4) . . ?
O21 Si5 O4 110.4(4) . . ?
O14 Si5 O5 117.1(4) . . ?
O21 Si5 O5 106.6(4) . . ?
O4 Si5 O5 106.1(4) . . ?
O19 Si6 O6 118.0(4) . . ?
O19 Si6 O18 108.6(4) . . ?
O6 Si6 O18 105.9(4) . . ?
O19 Si6 O5 108.1(4) . . ?
O6 Si6 O5 113.7(5) . . ?
O18 Si6 O5 101.0(4) . . ?
O22 Si7 O7 110.2(4) 6_655 . ?
O22 Si7 O17 114.8(5) 6_655 . ?
O7 Si7 O17 113.4(4) . . ?
O22 Si7 O23 104.4(5) 6_655 . ?
O7 Si7 O23 109.5(5) . . ?
O17 Si7 O23 103.8(5) . . ?
O12 Si8 O8 114.7(4) . . ?
O12 Si8 O13 108.3(4) . . ?
O8 Si8 O13 107.9(4) . . ?
O12 Si8 O7 110.9(4) . . ?
O8 Si8 O7 107.8(4) . . ?
O13 Si8 O7 106.9(4) . . ?
O8 Si9 O9 106.2(4) . . ?
O8 Si9 O25 115.0(5) . . ?
O9 Si9 O25 120.2(5) . . ?
O8 Si9 O18 103.9(4) . 2 ?
O9 Si9 O18 108.6(4) . 2 ?
O25 Si9 O18 101.6(5) . 2 ?
O15 Si10 O10 111.0(4) 2 . ?
O15 Si10 O26 105.6(5) 2 . ?
O10 Si10 O26 110.0(5) . . ?
O15 Si10 O9 110.8(5) 2 . ?
O10 Si10 O9 107.5(4) . . ?
O26 Si10 O9 111.9(5) . . ?
O14 Si11 O11 108.6(4) . . ?
O14 Si11 O10 109.2(4) . . ?
O11 Si11 O10 115.5(4) . . ?
O14 Si11 O22 115.6(4) . . ?
O11 Si11 O22 102.6(4) . . ?
O10 Si11 O22 105.4(4) . . ?
O12 Si12 O11 109.1(4) . . ?
O12 Si12 O24 102.3(5) . . ?
O11 Si12 O24 119.2(5) . . ?
O12 Si12 O20 109.8(4) . . ?
O11 Si12 O20 110.4(4) . . ?
O24 Si12 O20 105.6(5) . . ?
Si2 O1 Si1 153.6(6) . . ?
Si2 O2 Si3 143.6(5) . . ?
Si3 O3 Si4 174.2(6) . . ?
Si4 O4 Si5 151.3(5) . . ?
Si5 O5 Si6 144.4(5) . . ?
Si6 O6 Si2 145.5(5) . . ?
Si7 O7 Si8 157.2(5) . . ?
Si8 O8 Si9 151.7(6) . . ?
Si9 O9 Si10 145.5(6) . . ?
Si10 O10 Si11 158.4(6) . . ?
Si12 O11 Si11 149.9(5) . . ?
Si8 O12 Si12 164.8(5) . . ?
Si2 O13 Si8 174.6(6) . . ?
Si5 O14 Si11 162.1(6) . . ?
Si10 O15 Si1 146.4(6) 2_554 . ?
Si4 O16 Si1 171.1(6) 2_554 . ?
Si7 O17 Si4 138.7(5) . 2_554 ?
Si6 O18 Si9 143.1(6) . 2_554 ?
Si3 O19 Si6 157.0(6) 2_554 . ?
Si12 O20 Si3 145.3(5) . 2_554 ?
Si1 O21 Si5 146.5(6) 6 . ?
Si7 O22 Si11 148.5(6) 6 . ?
Si7 O23 Si7 154.6(7) . 8 ?
Si12 O24 Si12 145.9(8) . 8 ?
Si9 O25 Si9 137.3(7) 8 . ?
Si10 O26 Si10 142.6(8) 8 . ?

_refine_diff_density_max         0.65
_refine_diff_density_min         -0.41
_refine_diff_density_rms         0.34
