#------------------------------------------------------------------------------
#$Date: 2024-08-05 20:07:46 +0200 (Mon 05 de Aug de 2024) $
#$Revision: 293767 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/20/1572015.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_1572015
loop_
_publ_author_name
'Bao, Ming'
'Bohórquez, Arnold R Romero'
'Arman, Hadi'
'Doyle, Michael P.'
_publ_section_title
;
 Photoinduced [4 + 2]-cycloaddition reactions of vinyldiazo compounds for
 the construction of heterocyclic and bicyclic rings.
;
_journal_issue                   30
_journal_name_full               'Chemical science'
_journal_page_first              12042
_journal_page_last               12046
_journal_paper_doi               10.1039/d4sc03558e
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C35 H41 N3 O4 Si'
_chemical_formula_sum            'C35 H41 N3 O4 Si'
_chemical_formula_weight         595.80
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-03
_audit_creation_method
;
Olex2 1.5-ac5-024
(compiled 2022.04.12 svn.rca3783a0 for Rigaku Oxford Diffraction, GUI svn.r6498)
;
_audit_update_record
;
2024-04-05 deposited with the CCDC.	2024-06-27 downloaded from the CCDC.
;
_cell_angle_alpha                90.5720(10)
_cell_angle_beta                 92.7850(10)
_cell_angle_gamma                107.3760(10)
_cell_formula_units_Z            4
_cell_length_a                   14.0714(2)
_cell_length_b                   14.8588(2)
_cell_length_c                   16.3784(2)
_cell_measurement_reflns_used    23130
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      75.9960
_cell_measurement_theta_min      4.1390
_cell_volume                     3263.25(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_collection       'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_data_reduction        'CrysAlisPro 1.171.42.102a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac5-024 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -122.00 -30.00   0.50    0.42    --  -46.65 -16.00  72.00  184
  2  ω     30.00 123.00   0.50    0.42    --   46.65  16.00-118.00  186
  3  ω    -28.00  29.00   0.50    0.42    --   46.65 -16.00  72.00  114
  4  ω   -167.00 -75.00   0.50    1.66    --  -91.75 -16.00  72.00  184
  5  ω     90.00 178.00   0.50    1.66    --  106.91  16.00-118.00  176
  6  ω   -118.00 -83.00   0.50    0.42    --  -46.65 -57.00 120.00   70
  7  ω    -29.00  30.00   0.50    0.42    --  -46.65  16.00-118.00  118
  8  ω   -118.00 -83.00   0.50    0.42    --  -46.65 -57.00   0.00   70
  9  ω    -30.00  29.00   0.50    0.42    --  -46.65  19.00 -60.00  118
 10  ω    -86.00 -13.00   0.50    0.42    --  -46.65 125.00-120.00  146
 11  ω     83.00 120.00   0.50    0.42    --   46.65  57.00   0.00   74
 12  ω    -25.00  63.00   0.50    0.42    --   46.65 -57.00  60.00  176
 13  ω     34.00  93.00   0.50    0.42    --   46.65-125.00 120.00  118
 14  ω    -51.00 -19.00   0.50    1.66    --  -91.75  45.00-150.00   64
 15  ω    -51.00 -19.00   0.50    1.66    --  -91.75  45.00  60.00   64
 16  ω   -164.00-100.00   0.50    1.66    --  -91.75 -94.00 150.00  128
 17  ω    -51.00 -19.00   0.50    1.66    --  -91.75  45.00-180.00   64
 18  ω    -51.00 -19.00   0.50    1.66    --  -91.75  45.00-120.00   64
 19  ω   -164.00 -90.00   0.50    1.66    --  -91.75 -60.00-110.28  148
 20  ω   -164.00-101.00   0.50    1.66    --  -91.75 -77.00-180.00  126
 21  ω   -162.00 -87.00   0.50    1.66    --  -91.75-125.00-180.00  150
 22  ω   -101.00 -19.00   0.50    1.66    --  -91.75  77.00  30.00  164
 23  ω   -164.00-101.00   0.50    1.66    --  -91.75 -77.00-150.00  126
 24  ω   -164.00-100.00   0.50    1.66    --  -91.75 -94.00  60.00  128
 25  ω    -85.00 -22.00   0.50    1.66    --  -91.75 125.00 -60.00  126
 26  ω    -71.00 -19.00   0.50    1.66    --  -91.75  61.00 120.00  104
 27  ω     34.00  71.00   0.50    1.66    --  106.91 -61.00 120.00   74
 28  ω     37.00 112.00   0.50    1.66    --  106.91-125.00  60.00  150
 29  ω     37.00 112.00   0.50    1.66    --  106.91-125.00 120.00  150
 30  ω     37.00 112.00   0.50    1.66    --  106.91-125.00  30.00  150
 31  ω     34.00 106.00   0.50    1.66    --  106.91 -94.00-120.00  144
 32  ω     34.00 106.00   0.50    1.66    --  106.91 -94.00 150.00  144
 33  ω     34.00  71.00   0.50    1.66    --  106.91 -61.00  60.00   74
 34  ω     37.00 112.00   0.50    1.66    --  106.91-125.00-180.00  150
 35  ω     38.00 108.00   0.50    1.66    --  106.91-111.00 -62.55  140
 36  ω     34.00 106.00   0.50    1.66    --  106.91 -94.00-180.00  144
 37  ω     37.00 112.00   0.50    1.66    --  106.91-125.00 -30.00  150
 38  ω     34.00  71.00   0.50    1.66    --  106.91 -61.00-120.00   74
 39  ω     34.00 106.00   0.50    1.66    --  106.91 -94.00  30.00  144
 40  ω     34.00  71.00   0.50    1.66    --  106.91 -61.00-150.00   74
 41  ω     39.00 119.00   0.50    1.66    --  106.91-134.00 -95.97  160
 42  ω     92.00 178.00   0.50    1.66    --  106.91  30.00 -30.00  172
 43  ω     34.00  71.00   0.50    1.66    --  106.91 -61.00  30.00   74
 44  ω     34.00 106.00   0.50    1.66    --  106.91 -94.00  90.00  144
 45  ω   -118.00 -31.00   0.50    0.42    --  -46.65 -55.00  26.88  174
 46  ω     31.00 120.00   0.50    0.42    --   46.65  55.00 158.42  178
 47  ω     31.00 120.00   0.50    0.42    --   46.65  54.00  -6.07  178
 48  ω     31.00 120.00   0.50    0.42    --   46.65  55.00-134.99  178
 49  ω     31.00 120.00   0.50    0.42    --   46.65  55.00 115.64  178
 50  ω     31.00 120.00   0.50    0.42    --   46.65  53.00 -74.43  178
;
_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      -0.0591211000
_diffrn_orient_matrix_UB_12      -0.1024211000
_diffrn_orient_matrix_UB_13      0.0181468000
_diffrn_orient_matrix_UB_21      0.0950006000
_diffrn_orient_matrix_UB_22      -0.0299968000
_diffrn_orient_matrix_UB_23      -0.0077993000
_diffrn_orient_matrix_UB_31      0.0260408000
_diffrn_orient_matrix_UB_32      0.0204948000
_diffrn_orient_matrix_UB_33      0.0921092000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0143
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23211
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.829
_diffrn_reflns_theta_min         2.702
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.966
_exptl_absorpt_correction_T_max  0.117
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.102a (Rigaku Oxford Diffraction, 2023)
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_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.213
_exptl_crystal_description       plate
_exptl_crystal_F_000             1272
_exptl_crystal_size_max          0.139
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.062
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.567
_refine_diff_density_rms         0.054
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         23211
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0669
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0300P)²+3.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1395
_refine_ls_wR_factor_ref         0.1432
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20241
_reflns_number_total             23211
_reflns_threshold_expression     'I > 2σ(I)'
_twin_special_details
;
Component 2 rotated by 179.5296° 
around [-0.00 -0.00 1.00] (reciprocal) or [0.06 0.03 1.00] (direct)
;
_cod_data_source_file            d4sc03558e2.cif
_cod_data_source_block           hpd873_twin1_hklf4
_cod_depositor_comments
'Adding full bibliography for 1572014--1572015.cif.'
_cod_database_code               1572015
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H O N Si'
_chemical_oxdiff_usercomment     627
_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.
;
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5668(7)
 0.4332(7)
2. 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
3.a Ternary CH refined with riding coordinates:
 C4(H4), C39(H39)
3.b Secondary CH2 refined with riding coordinates:
 C37(H37A,H37B), C2(H2A,H2B), C55(H55A,H55B), C56(H56A,H56B), C20(H20A,H20B),
 C21(H21A,H21B)
3.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C64(H64), C18(H18), C53(H53), C43(H43), C29(H29), C47(H47), C8(H8),
 C44(H44), C12(H12), C16(H16), C45(H45), C23(H23), C17(H17), C50(H50), C9(H9),
 C27(H27), C62(H62), C49(H49), C58(H58), C15(H15), C10(H10), C46(H46), C61(H61),
  C60(H60), C51(H51), C52(H52), C24(H24), C26(H26), C11(H11), C25(H25), C59(H59)
3.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C68(H68A,H68B,H68C), C28(H28A,H28B,H28C), C33(H33A,H33B,
 H33C), C70(H70A,H70B,H70C), C69(H69A,H69B,H69C), C34(H34A,H34B,H34C), C31(H31A,
 H31B,H31C), C66(H66A,H66B,H66C), C30(H30A,H30B,H30C), C35(H35A,H35B,H35C),
 C65(H65A,H65B,H65C)
;
_olex2_exptl_crystal_mounting_method 'nylon loop'
_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 2.083
_oxdiff_exptl_absorpt_empirical_full_min 0.472
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.22506(7) 0.82634(7) 0.41650(6) 0.0547(2) Uani 1 1 d . . . . .
Si2 Si 0.75497(7) 0.80130(7) 1.10785(6) 0.0539(2) Uani 1 1 d . . . . .
O3 O 0.15555(15) 0.32425(14) 0.56219(12) 0.0477(5) Uani 1 1 d . . . . .
O6 O 0.59556(16) 0.43989(15) 1.00619(12) 0.0493(5) Uani 1 1 d . . . . .
O7 O 0.63941(15) 0.32113(14) 0.94961(12) 0.0468(5) Uani 1 1 d . . . . .
O5 O 0.70239(15) 0.72575(15) 0.79559(13) 0.0499(5) Uani 1 1 d . . . . .
O2 O 0.09800(16) 0.43106(15) 0.49703(12) 0.0507(5) Uani 1 1 d . . . . .
O4 O 0.17024(16) 0.71576(15) 0.44348(13) 0.0534(5) Uani 1 1 d . . . . .
O8 O 0.67427(16) 0.72722(15) 1.04132(13) 0.0508(5) Uani 1 1 d . . . . .
O1 O 0.22540(16) 0.74536(16) 0.69292(14) 0.0566(5) Uani 1 1 d . . . . .
N2 N 0.39381(18) 0.62613(18) 0.63513(14) 0.0447(5) Uani 1 1 d . . . . .
N1 N 0.30203(18) 0.63991(18) 0.65419(14) 0.0455(6) Uani 1 1 d . . . . .
N4 N 0.77937(18) 0.62107(17) 0.83920(14) 0.0436(5) Uani 1 1 d . . . . .
N5 N 0.87179(17) 0.60637(17) 0.86026(14) 0.0428(5) Uani 1 1 d . . . . .
N6 N 0.72106(19) 0.68166(18) 0.98530(15) 0.0474(6) Uani 1 1 d . . . . .
N3 N 0.2239(2) 0.68735(19) 0.50940(15) 0.0506(6) Uani 1 1 d . . . . .
C54 C 0.6361(2) 0.4103(2) 0.95319(18) 0.0433(6) Uani 1 1 d . . . . .
C1 C 0.3916(2) 0.5384(2) 0.63322(17) 0.0444(6) Uani 1 1 d . . . . .
C36 C 0.8678(2) 0.5185(2) 0.86644(17) 0.0431(6) Uani 1 1 d . . . . .
C38 C 0.6832(2) 0.4640(2) 0.88178(17) 0.0426(6) Uani 1 1 d . . . . .
C3 C 0.2043(2) 0.4765(2) 0.61954(17) 0.0444(6) Uani 1 1 d . . . . .
C41 C 0.7801(2) 0.7045(2) 0.80300(17) 0.0447(6) Uani 1 1 d . . . . .
C6 C 0.3034(2) 0.7257(2) 0.68818(18) 0.0487(7) Uani 1 1 d . . . . .
C19 C 0.1481(2) 0.4118(2) 0.55230(18) 0.0446(6) Uani 1 1 d . . . . .
C57 C 0.7108(2) 0.1664(2) 1.01617(18) 0.0464(7) Uani 1 1 d . . . . .
C42 C 0.8744(2) 0.7642(2) 0.76943(17) 0.0450(6) Uani 1 1 d . . . . .
C13 C 0.4864(2) 0.5192(2) 0.61637(17) 0.0445(7) Uani 1 1 d . . . . .
C7 C 0.3994(2) 0.7897(2) 0.72484(18) 0.0477(7) Uani 1 1 d . . . . .
C40 C 0.6894(2) 0.5679(2) 0.87674(17) 0.0423(6) Uani 1 1 d . . . . .
C5 C 0.2084(2) 0.5808(2) 0.61785(18) 0.0455(7) Uani 1 1 d . . . . .
C4 C 0.1415(2) 0.5161(2) 0.67524(18) 0.0472(7) Uani 1 1 d . . . . .
H4 H 0.168120 0.525152 0.733444 0.057 Uiso 1 1 calc R U . . .
C48 C 0.9645(2) 0.5001(2) 0.88600(17) 0.0444(6) Uani 1 1 d . . . . .
C37 C 0.7726(2) 0.4408(2) 0.84845(19) 0.0474(7) Uani 1 1 d . . . . .
H37A H 0.778418 0.381960 0.873037 0.057 Uiso 1 1 calc R U . . .
H37B H 0.761647 0.429752 0.788549 0.057 Uiso 1 1 calc R U . . .
C14 C 0.4879(2) 0.4294(2) 0.59077(18) 0.0492(7) Uani 1 1 d . . . . .
H14 H 0.427306 0.379466 0.583746 0.059 Uiso 1 1 calc R U . . .
C64 C 0.6565(2) 0.6196(2) 0.94246(17) 0.0431(6) Uani 1 1 d . . . . .
H64 H 0.587723 0.606131 0.952125 0.052 Uiso 1 1 calc R U . . .
C18 C 0.5766(2) 0.5908(2) 0.62651(18) 0.0489(7) Uani 1 1 d . . . . .
H18 H 0.576880 0.651979 0.644117 0.059 Uiso 1 1 calc R U . . .
C2 C 0.3004(2) 0.4616(2) 0.65486(19) 0.0478(7) Uani 1 1 d . . . . .
H2A H 0.298229 0.458747 0.715122 0.057 Uiso 1 1 calc R U . . .
H2B H 0.305121 0.400319 0.634195 0.057 Uiso 1 1 calc R U . . .
C53 C 0.9681(2) 0.4130(2) 0.91543(18) 0.0470(7) Uani 1 1 d . . . . .
H53 H 0.908009 0.364051 0.922794 0.056 Uiso 1 1 calc R U . . .
C43 C 0.9346(2) 0.7284(2) 0.72209(18) 0.0481(7) Uani 1 1 d . . . . .
H43 H 0.920370 0.662059 0.714753 0.058 Uiso 1 1 calc R U . . .
C22 C 0.2227(2) 0.1650(2) 0.49935(19) 0.0484(7) Uani 1 1 d . . . . .
C55 C 0.5885(2) 0.2610(2) 1.0130(2) 0.0509(7) Uani 1 1 d . . . . .
H55A H 0.516486 0.255370 1.009193 0.061 Uiso 1 1 calc R U . . .
H55B H 0.616459 0.287814 1.067671 0.061 Uiso 1 1 calc R U . . .
C29 C 0.1663(2) 0.6208(2) 0.54773(18) 0.0460(7) Uani 1 1 d . . . . .
H29 H 0.097413 0.597216 0.531600 0.055 Uiso 1 1 calc R U . . .
C47 C 0.8960(2) 0.8618(2) 0.77983(19) 0.0494(7) Uani 1 1 d . . . . .
H47 H 0.854880 0.887179 0.811567 0.059 Uiso 1 1 calc R U . . .
C56 C 0.6037(2) 0.1650(2) 1.0002(2) 0.0510(7) Uani 1 1 d . . . . .
H56A H 0.561140 0.119584 1.037043 0.061 Uiso 1 1 calc R U . . .
H56B H 0.581997 0.142548 0.943209 0.061 Uiso 1 1 calc R U . . .
C8 C 0.4646(2) 0.7584(2) 0.77537(18) 0.0498(7) Uani 1 1 d . . . . .
H8 H 0.454666 0.692717 0.780856 0.060 Uiso 1 1 calc R U . . .
C44 C 1.0151(2) 0.7884(2) 0.68555(18) 0.0522(7) Uani 1 1 d . . . . .
H44 H 1.055739 0.763336 0.653093 0.063 Uiso 1 1 calc R U . . .
C12 C 0.4155(3) 0.8858(2) 0.7158(2) 0.0557(8) Uani 1 1 d . . . . .
H12 H 0.370948 0.907814 0.681862 0.067 Uiso 1 1 calc R U . . .
C16 C 0.6662(2) 0.4847(2) 0.58631(18) 0.0525(7) Uani 1 1 d . . . . .
H16 H 0.727461 0.472859 0.576555 0.063 Uiso 1 1 calc R U . . .
C20 C 0.0966(2) 0.2545(2) 0.50317(19) 0.0509(7) Uani 1 1 d . . . . .
H20A H 0.114146 0.274686 0.447005 0.061 Uiso 1 1 calc R U . . .
H20B H 0.024775 0.246619 0.508299 0.061 Uiso 1 1 calc R U . . .
C45 C 1.0365(2) 0.8851(3) 0.69617(19) 0.0558(8) Uani 1 1 d . . . . .
H45 H 1.091573 0.926465 0.670863 0.067 Uiso 1 1 calc R U . . .
C39 C 0.6136(2) 0.4966(2) 0.82237(17) 0.0447(6) Uani 1 1 d . . . . .
H39 H 0.632013 0.497020 0.764136 0.054 Uiso 1 1 calc R U . . .
C23 C 0.2465(2) 0.1617(2) 0.41817(19) 0.0519(7) Uani 1 1 d . . . . .
H23 H 0.196618 0.158053 0.375960 0.062 Uiso 1 1 calc R U . . .
C17 C 0.6658(2) 0.5741(2) 0.61132(18) 0.0515(7) Uani 1 1 d . . . . .
H17 H 0.726732 0.623779 0.618001 0.062 Uiso 1 1 calc R U . . .
C50 C 1.1445(2) 0.5548(2) 0.89396(18) 0.0490(7) Uani 1 1 d . . . . .
H50 H 1.204881 0.603465 0.886934 0.059 Uiso 1 1 calc R U . . .
C63 C 0.5029(2) 0.4740(2) 0.83204(18) 0.0480(7) Uani 1 1 d . . . . .
H63A H 0.467914 0.415085 0.802055 0.072 Uiso 1 1 calc R U . . .
H63B H 0.479568 0.525327 0.810212 0.072 Uiso 1 1 calc R U . . .
H63C H 0.489271 0.466907 0.890118 0.072 Uiso 1 1 calc R U . . .
C9 C 0.5443(2) 0.8231(2) 0.81792(19) 0.0544(8) Uani 1 1 d . . . . .
H9 H 0.587916 0.801506 0.853293 0.065 Uiso 1 1 calc R U . . .
C27 C 0.2967(3) 0.1701(2) 0.5600(2) 0.0552(8) Uani 1 1 d . . . . .
H27 H 0.282050 0.172259 0.615900 0.066 Uiso 1 1 calc R U . . .
C21 C 0.1186(2) 0.1623(2) 0.5200(2) 0.0544(8) Uani 1 1 d . . . . .
H21A H 0.109980 0.147990 0.578591 0.065 Uiso 1 1 calc R U . . .
H21B H 0.069892 0.110896 0.487582 0.065 Uiso 1 1 calc R U . . .
C62 C 0.7537(3) 0.1799(2) 1.09529(19) 0.0521(7) Uani 1 1 d . . . . .
H62 H 0.715672 0.189621 1.139073 0.062 Uiso 1 1 calc R U . . .
C49 C 1.0535(2) 0.5701(2) 0.87542(18) 0.0487(7) Uani 1 1 d . . . . .
H49 H 1.051975 0.629410 0.855181 0.058 Uiso 1 1 calc R U . . .
C68 C 0.5862(3) 0.8113(2) 1.1877(2) 0.0591(8) Uani 1 1 d . . . . .
H68A H 0.545957 0.766393 1.145936 0.089 Uiso 1 1 calc R U . . .
H68B H 0.547136 0.850719 1.207910 0.089 Uiso 1 1 calc R U . . .
H68C H 0.605217 0.776701 1.233112 0.089 Uiso 1 1 calc R U . . .
C58 C 0.7675(2) 0.1523(2) 0.95375(19) 0.0534(8) Uani 1 1 d . . . . .
H58 H 0.739443 0.142996 0.899233 0.064 Uiso 1 1 calc R U . . .
C15 C 0.5776(3) 0.4133(2) 0.57568(19) 0.0541(8) Uani 1 1 d . . . . .
H15 H 0.577889 0.352335 0.557831 0.065 Uiso 1 1 calc R U . . .
C10 C 0.5600(3) 0.9185(3) 0.8088(2) 0.0580(8) Uani 1 1 d . . . . .
H10 H 0.613914 0.962807 0.838328 0.070 Uiso 1 1 calc R U . . .
C46 C 0.9771(2) 0.9212(2) 0.7439(2) 0.0547(8) Uani 1 1 d . . . . .
H46 H 0.992403 0.987555 0.751973 0.066 Uiso 1 1 calc R U . . .
C61 C 0.8509(3) 0.1792(2) 1.1112(2) 0.0562(8) Uani 1 1 d . . . . .
H61 H 0.879078 0.188458 1.165607 0.067 Uiso 1 1 calc R U . . .
C28 C 0.0293(2) 0.4893(2) 0.6664(2) 0.0521(7) Uani 1 1 d . . . . .
H28A H 0.007289 0.473410 0.608924 0.078 Uiso 1 1 calc R U . . .
H28B H 0.007106 0.542388 0.684546 0.078 Uiso 1 1 calc R U . . .
H28C H 0.000497 0.434542 0.699903 0.078 Uiso 1 1 calc R U . . .
C60 C 0.9066(3) 0.1652(3) 1.0488(2) 0.0606(8) Uani 1 1 d . . . . .
H60 H 0.973491 0.165057 1.059793 0.073 Uiso 1 1 calc R U . . .
C51 C 1.1469(2) 0.4673(2) 0.92304(18) 0.0513(7) Uani 1 1 d . . . . .
H51 H 1.209024 0.456042 0.935253 0.062 Uiso 1 1 calc R U . . .
C67 C 0.6799(3) 0.8737(2) 1.1504(2) 0.0562(8) Uani 1 1 d . . . . .
C52 C 1.0594(3) 0.3980(2) 0.93385(19) 0.0517(7) Uani 1 1 d . . . . .
H52 H 1.061298 0.338869 0.954217 0.062 Uiso 1 1 calc R U . . .
C24 C 0.3411(3) 0.1635(2) 0.3976(2) 0.0572(8) Uani 1 1 d . . . . .
H24 H 0.356099 0.161182 0.341869 0.069 Uiso 1 1 calc R U . . .
C32 C 0.1637(3) 0.8335(2) 0.3139(2) 0.0554(8) Uani 1 1 d . . . . .
C26 C 0.3912(3) 0.1719(3) 0.5398(2) 0.0606(8) Uani 1 1 d . . . . .
H26 H 0.441166 0.175386 0.581869 0.073 Uiso 1 1 calc R U . . .
C33 C 0.2086(3) 0.9312(2) 0.2787(2) 0.0569(8) Uani 1 1 d . . . . .
H33A H 0.194188 0.978994 0.313581 0.085 Uiso 1 1 calc R U . . .
H33B H 0.179392 0.932790 0.223394 0.085 Uiso 1 1 calc R U . . .
H33C H 0.280945 0.944396 0.276642 0.085 Uiso 1 1 calc R U . . .
C70 C 0.7441(3) 0.9441(2) 1.2148(2) 0.0594(8) Uani 1 1 d . . . . .
H70A H 0.764788 0.909663 1.259663 0.089 Uiso 1 1 calc R U . . .
H70B H 0.705416 0.983182 1.236221 0.089 Uiso 1 1 calc R U . . .
H70C H 0.803354 0.984482 1.189904 0.089 Uiso 1 1 calc R U . . .
C11 C 0.4971(3) 0.9495(3) 0.7566(2) 0.0618(9) Uani 1 1 d . . . . .
H11 H 0.509749 1.015156 0.748441 0.074 Uiso 1 1 calc R U . . .
C69 C 0.6494(3) 0.9295(3) 1.0800(2) 0.0629(9) Uani 1 1 d . . . . .
H69A H 0.709361 0.971370 1.057153 0.094 Uiso 1 1 calc R U . . .
H69B H 0.608986 0.967261 1.100952 0.094 Uiso 1 1 calc R U . . .
H69C H 0.610435 0.885427 1.037191 0.094 Uiso 1 1 calc R U . . .
C25 C 0.4141(3) 0.1688(3) 0.4590(2) 0.0606(8) Uani 1 1 d . . . . .
H25 H 0.479420 0.170243 0.445571 0.073 Uiso 1 1 calc R U . . .
C59 C 0.8651(3) 0.1514(3) 0.9697(2) 0.0618(9) Uani 1 1 d . . . . .
H59 H 0.903308 0.141241 0.926166 0.074 Uiso 1 1 calc R U . . .
C34 C 0.0520(3) 0.8105(3) 0.3158(2) 0.0656(9) Uani 1 1 d . . . . .
H34A H 0.024362 0.747598 0.337976 0.098 Uiso 1 1 calc R U . . .
H34B H 0.023421 0.811733 0.260202 0.098 Uiso 1 1 calc R U . . .
H34C H 0.035518 0.857300 0.350494 0.098 Uiso 1 1 calc R U . . .
C31 C 0.1982(3) 0.9078(3) 0.4948(2) 0.0695(10) Uani 1 1 d . . . . .
H31A H 0.126930 0.901941 0.491210 0.104 Uiso 1 1 calc R U . . .
H31B H 0.236803 0.972962 0.484394 0.104 Uiso 1 1 calc R U . . .
H31C H 0.217048 0.890787 0.549605 0.104 Uiso 1 1 calc R U . . .
C66 C 0.8663(3) 0.8706(3) 1.0581(3) 0.0769(11) Uani 1 1 d . . . . .
H66A H 0.897625 0.827953 1.031872 0.115 Uiso 1 1 calc R U . . .
H66B H 0.913530 0.910770 1.099094 0.115 Uiso 1 1 calc R U . . .
H66C H 0.847287 0.910161 1.016735 0.115 Uiso 1 1 calc R U . . .
C30 C 0.3600(3) 0.8531(3) 0.4136(3) 0.0785(12) Uani 1 1 d . . . . .
H30A H 0.388166 0.846105 0.468254 0.118 Uiso 1 1 calc R U . . .
H30B H 0.388613 0.918064 0.396118 0.118 Uiso 1 1 calc R U . . .
H30C H 0.375781 0.809556 0.374961 0.118 Uiso 1 1 calc R U . . .
C35 C 0.1840(3) 0.7575(3) 0.2563(2) 0.0704(10) Uani 1 1 d . . . . .
H35A H 0.256033 0.770761 0.251804 0.106 Uiso 1 1 calc R U . . .
H35B H 0.152205 0.759282 0.202020 0.106 Uiso 1 1 calc R U . . .
H35C H 0.156443 0.694871 0.279024 0.106 Uiso 1 1 calc R U . . .
C65 C 0.7919(3) 0.7302(3) 1.1906(2) 0.0732(11) Uani 1 1 d . . . . .
H65A H 0.732545 0.694572 1.218226 0.110 Uiso 1 1 calc R U . . .
H65B H 0.839153 0.772579 1.230307 0.110 Uiso 1 1 calc R U . . .
H65C H 0.823407 0.686343 1.166597 0.110 Uiso 1 1 calc R U . . .
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'
N N 0.0311 0.0180 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 10 0.0585
8 -7 -1 0.0543
-1 -2 -10 0.0694
-8 7 1 0.0374
-1 -2 10 0.0594
-4 -7 -1 0.0177
2 3 -10 0.0628
4 7 1 0.0432
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Si1 C32 103.40(14) . . ?
O4 Si1 C31 107.91(15) . . ?
O4 Si1 C30 112.45(16) . . ?
C32 Si1 C31 112.29(16) . . ?
C30 Si1 C32 112.71(18) . . ?
C30 Si1 C31 108.0(2) . . ?
O8 Si2 C67 103.41(13) . . ?
O8 Si2 C66 111.44(16) . . ?
O8 Si2 C65 108.35(16) . . ?
C67 Si2 C65 109.98(17) . . ?
C66 Si2 C67 113.87(17) . . ?
C66 Si2 C65 109.5(2) . . ?
C19 O3 C20 114.8(2) . . ?
C54 O7 C55 115.2(2) . . ?
N3 O4 Si1 112.38(18) . . ?
N6 O8 Si2 113.42(17) . . ?
C1 N2 N1 113.7(3) . . ?
N2 N1 C5 121.4(2) . . ?
C6 N1 N2 118.4(3) . . ?
C6 N1 C5 117.5(2) . . ?
N5 N4 C40 121.0(2) . . ?
C41 N4 N5 118.0(2) . . ?
C41 N4 C40 117.9(2) . . ?
C36 N5 N4 114.3(2) . . ?
C64 N6 O8 110.7(2) . . ?
C29 N3 O4 110.6(3) . . ?
O6 C54 O7 123.0(3) . . ?
O6 C54 C38 125.9(3) . . ?
O7 C54 C38 111.0(2) . . ?
N2 C1 C13 116.4(3) . . ?
N2 C1 C2 121.2(3) . . ?
C13 C1 C2 122.1(3) . . ?
N5 C36 C48 115.8(3) . . ?
N5 C36 C37 121.5(3) . . ?
C48 C36 C37 122.6(3) . . ?
C54 C38 C40 118.5(2) . . ?
C54 C38 C37 117.7(2) . . ?
C54 C38 C39 116.1(2) . . ?
C40 C38 C37 113.7(2) . . ?
C40 C38 C39 59.07(18) . . ?
C37 C38 C39 118.7(2) . . ?
C19 C3 C5 119.0(2) . . ?
C19 C3 C4 115.6(2) . . ?
C19 C3 C2 118.0(2) . . ?
C4 C3 C5 58.73(19) . . ?
C2 C3 C5 113.0(2) . . ?
C2 C3 C4 119.1(2) . . ?
O5 C41 N4 119.4(3) . . ?
O5 C41 C42 121.6(3) . . ?
N4 C41 C42 118.9(2) . . ?
O1 C6 N1 119.8(3) . . ?
O1 C6 C7 120.9(3) . . ?
N1 C6 C7 119.1(3) . . ?
O3 C19 C3 110.8(2) . . ?
O2 C19 O3 122.7(3) . . ?
O2 C19 C3 126.4(3) . . ?
C62 C57 C56 120.2(3) . . ?
C58 C57 C56 121.4(3) . . ?
C58 C57 C62 118.4(3) . . ?
C43 C42 C41 123.4(3) . . ?
C43 C42 C47 119.3(3) . . ?
C47 C42 C41 116.9(3) . . ?
C14 C13 C1 121.3(3) . . ?
C18 C13 C1 120.2(3) . . ?
C18 C13 C14 118.5(3) . . ?
C8 C7 C6 123.1(3) . . ?
C12 C7 C6 116.8(3) . . ?
C12 C7 C8 119.6(3) . . ?
N4 C40 C38 111.1(2) . . ?
N4 C40 C64 114.9(2) . . ?
N4 C40 C39 116.3(2) . . ?
C64 C40 C38 122.9(2) . . ?
C64 C40 C39 120.3(3) . . ?
C39 C40 C38 60.69(19) . . ?
N1 C5 C3 110.8(2) . . ?
N1 C5 C4 115.5(2) . . ?
N1 C5 C29 115.7(3) . . ?
C4 C5 C3 60.47(19) . . ?
C29 C5 C3 122.1(3) . . ?
C29 C5 C4 120.9(3) . . ?
C5 C4 C3 60.80(19) . . ?
C5 C4 C28 123.0(3) . . ?
C28 C4 C3 123.4(3) . . ?
C53 C48 C36 121.3(3) . . ?
C49 C48 C36 120.0(3) . . ?
C49 C48 C53 118.8(3) . . ?
C36 C37 C38 112.0(3) . . ?
C15 C14 C13 120.2(3) . . ?
N6 C64 C40 119.3(3) . . ?
C17 C18 C13 121.0(3) . . ?
C1 C2 C3 112.7(3) . . ?
C52 C53 C48 120.0(3) . . ?
C44 C43 C42 120.5(3) . . ?
C23 C22 C21 120.2(3) . . ?
C27 C22 C23 118.4(3) . . ?
C27 C22 C21 121.4(3) . . ?
O7 C55 C56 107.2(2) . . ?
N3 C29 C5 118.8(3) . . ?
C46 C47 C42 119.8(3) . . ?
C57 C56 C55 112.9(3) . . ?
C7 C8 C9 120.1(3) . . ?
C43 C44 C45 120.1(3) . . ?
C11 C12 C7 119.7(3) . . ?
C15 C16 C17 119.8(3) . . ?
O3 C20 C21 107.7(2) . . ?
C44 C45 C46 119.7(3) . . ?
C40 C39 C38 60.25(18) . . ?
C40 C39 C63 122.4(3) . . ?
C63 C39 C38 123.2(3) . . ?
C24 C23 C22 121.3(3) . . ?
C18 C17 C16 119.9(3) . . ?
C49 C50 C51 119.7(3) . . ?
C10 C9 C8 120.0(3) . . ?
C26 C27 C22 120.5(3) . . ?
C22 C21 C20 112.7(3) . . ?
C61 C62 C57 120.9(3) . . ?
C50 C49 C48 121.0(3) . . ?
C57 C58 C59 120.8(3) . . ?
C16 C15 C14 120.6(3) . . ?
C9 C10 C11 119.7(3) . . ?
C47 C46 C45 120.6(3) . . ?
C60 C61 C62 120.3(3) . . ?
C61 C60 C59 119.6(3) . . ?
C52 C51 C50 119.7(3) . . ?
C68 C67 Si2 111.1(2) . . ?
C68 C67 C70 110.3(3) . . ?
C68 C67 C69 109.2(3) . . ?
C70 C67 Si2 109.4(2) . . ?
C70 C67 C69 108.5(3) . . ?
C69 C67 Si2 108.2(2) . . ?
C51 C52 C53 120.9(3) . . ?
C23 C24 C25 119.5(3) . . ?
C33 C32 Si1 110.1(2) . . ?
C33 C32 C35 109.1(3) . . ?
C34 C32 Si1 112.9(2) . . ?
C34 C32 C33 110.5(3) . . ?
C34 C32 C35 106.5(3) . . ?
C35 C32 Si1 107.6(2) . . ?
C27 C26 C25 120.7(3) . . ?
C10 C11 C12 120.7(3) . . ?
C26 C25 C24 119.6(3) . . ?
C60 C59 C58 120.0(3) . . ?
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 O4 1.668(2) . ?
Si1 C32 1.870(3) . ?
Si1 C31 1.881(4) . ?
Si1 C30 1.823(4) . ?
Si2 O8 1.673(2) . ?
Si2 C67 1.869(3) . ?
Si2 C66 1.832(4) . ?
Si2 C65 1.874(4) . ?
O3 C19 1.346(3) . ?
O3 C20 1.444(4) . ?
O6 C54 1.209(3) . ?
O7 C54 1.341(3) . ?
O7 C55 1.448(3) . ?
O5 C41 1.226(3) . ?
O2 C19 1.209(3) . ?
O4 N3 1.426(3) . ?
O8 N6 1.430(3) . ?
O1 C6 1.223(4) . ?
N2 N1 1.415(3) . ?
N2 C1 1.295(4) . ?
N1 C6 1.380(4) . ?
N1 C5 1.444(4) . ?
N4 N5 1.409(3) . ?
N4 C41 1.377(4) . ?
N4 C40 1.447(4) . ?
N5 C36 1.295(4) . ?
N6 C64 1.262(4) . ?
N3 C29 1.269(4) . ?
C54 C38 1.491(4) . ?
C1 C13 1.482(4) . ?
C1 C2 1.500(4) . ?
C36 C48 1.486(4) . ?
C36 C37 1.499(4) . ?
C38 C40 1.523(4) . ?
C38 C37 1.523(4) . ?
C38 C39 1.530(4) . ?
C3 C19 1.485(4) . ?
C3 C5 1.534(4) . ?
C3 C4 1.529(4) . ?
C3 C2 1.522(4) . ?
C41 C42 1.493(4) . ?
C6 C7 1.494(4) . ?
C57 C56 1.511(4) . ?
C57 C62 1.389(4) . ?
C57 C58 1.378(4) . ?
C42 C43 1.388(4) . ?
C42 C47 1.397(4) . ?
C13 C14 1.401(4) . ?
C13 C18 1.392(4) . ?
C7 C8 1.390(4) . ?
C7 C12 1.387(4) . ?
C40 C64 1.485(4) . ?
C40 C39 1.505(4) . ?
C5 C4 1.502(4) . ?
C5 C29 1.477(4) . ?
C4 C28 1.508(4) . ?
C48 C53 1.401(4) . ?
C48 C49 1.388(4) . ?
C14 C15 1.385(4) . ?
C18 C17 1.384(4) . ?
C53 C52 1.388(4) . ?
C43 C44 1.382(4) . ?
C22 C23 1.391(4) . ?
C22 C27 1.388(4) . ?
C22 C21 1.509(4) . ?
C55 C56 1.519(4) . ?
C47 C46 1.379(4) . ?
C8 C9 1.390(4) . ?
C44 C45 1.384(5) . ?
C12 C11 1.386(5) . ?
C16 C17 1.387(4) . ?
C16 C15 1.378(5) . ?
C20 C21 1.517(4) . ?
C45 C46 1.386(5) . ?
C39 C63 1.509(4) . ?
C23 C24 1.382(4) . ?
C50 C49 1.387(4) . ?
C50 C51 1.398(4) . ?
C9 C10 1.380(5) . ?
C27 C26 1.379(5) . ?
C62 C61 1.383(5) . ?
C68 C67 1.527(5) . ?
C58 C59 1.390(4) . ?
C10 C11 1.380(5) . ?
C61 C60 1.368(5) . ?
C60 C59 1.383(5) . ?
C51 C52 1.370(5) . ?
C67 C70 1.531(5) . ?
C67 C69 1.545(5) . ?
C24 C25 1.386(5) . ?
C32 C33 1.531(5) . ?
C32 C34 1.508(5) . ?
C32 C35 1.563(5) . ?
C26 C25 1.380(5) . ?
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
_oxdiff_twin_reflns_isolated
_oxdiff_twin_reflns_overlapped
_twin_individual_twin_lattice_type
_twin_individual_twin_matrix_11
_twin_individual_twin_matrix_12
_twin_individual_twin_matrix_13
_twin_individual_twin_matrix_21
_twin_individual_twin_matrix_22
_twin_individual_twin_matrix_23
_twin_individual_twin_matrix_31
_twin_individual_twin_matrix_32
_twin_individual_twin_matrix_33
1 0.5668(7) 39929 32442 ref 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000
0.0000 1.0000
2 0.4332(7) 39727 32442 nmt -1.0033 -0.0082 -0.0015 0.0090 -0.9975 -0.0013
0.1288 0.0578 0.9998
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
0.2322 1.9393 10.2822 -0.0258 -0.1163 0.9929
7.9065 -7.0463 -1.1386 0.2336 0.9714 -0.0434
-0.6136 -1.6137 -10.2960 0.0147 0.0704 -0.9974
-7.8818 7.0579 1.2969 -0.2334 -0.9706 0.0589
-0.7228 -1.6874 10.4466 0.4051 -0.0995 0.9088
-4.4561 -6.5510 -0.8074 0.9198 -0.2205 -0.3247
1.6509 3.0238 -9.8056 -0.5852 0.1426 -0.7982
4.4595 6.5646 0.6624 -0.9240 0.2216 0.3117
