#------------------------------------------------------------------------------
#$Date: 2025-08-19 00:06:14 +0300 (Tue, 19 Aug 2025) $
#$Revision: 301780 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557999.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_1557999
loop_
_publ_author_name
'Eichenberger, Sarah'
'Hönig, Moritz'
'Richter, Matthieu J. R.'
'Gershoni-Poranne, Renana'
'Carreira, Erick M.'
_publ_section_title
;
 Ring-fused cyclobutanes via cycloisomerization of alkylidenecyclopropane
 acylsilanes
;
_journal_issue                   20
_journal_name_full               'Chemical Science'
_journal_page_first              5294
_journal_page_last               5298
_journal_paper_doi               10.1039/D0SC02224A
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety         'C28 H30 Br N O2 Si, C3 H7'
_chemical_formula_sum            'C31 H37 Br N O2 Si'
_chemical_formula_weight         563.61
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-17 deposited with the CCDC.	2020-05-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.5460(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.00200(10)
_cell_length_b                   8.35050(10)
_cell_length_c                   18.65040(10)
_cell_measurement_reflns_used    57270
_cell_measurement_temperature    100.0(1)
_cell_measurement_theta_max      79.3500
_cell_measurement_theta_min      2.4230
_cell_volume                     2836.83(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.42a (Rigaku OD, 2019)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 300K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      1.00  33.00   0.50    0.17    --   34.00  96.00 116.03   64
  2  ω     29.00 120.00   0.50    0.17    --   54.00  81.00 101.51  182
  3  ω    120.00 175.00   0.50    0.68    --  110.00  77.00 120.00  110
  4  ω    131.00 168.00   0.50    0.68    --  110.00  77.00  60.00   74
  5  ω    118.00 175.00   0.50    0.68    --  110.00  77.00 150.00  114
  6  ω    121.00 175.00   0.50    0.68    --  110.00  77.00  30.00  108
  7  ω    120.00 176.00   0.50    0.68    --  110.00  77.00   0.00  112
  8  ω    125.00 176.00   0.50    0.68    --  110.00  77.00 -30.00  102
  9  ω     97.00 147.00   0.50    0.68    --  110.00  56.00 -17.60  100
 10  ω     94.00 138.00   0.50    0.68    --  110.00  57.00 -60.00   88
 11  ω     97.00 127.00   0.50    0.68    --  110.00  57.00 -30.00   60
 12  ω     97.00 178.00   0.50    0.68    --  110.00  57.00 -90.00  162
 13  ω     99.00 126.00   0.50    0.68    --  110.00  57.00-150.00   54
 14  ω     98.00 151.00   0.50    0.68    --  110.00  38.00-180.00  106
 15  ω     94.00 122.00   0.50    0.68    --  110.00  57.00-120.00   56
 16  ω    100.00 126.00   0.50    0.68    --  110.00  38.00-150.00   52
 17  ω     86.00 175.00   0.50    0.68    --  110.00  77.00-180.00  178
 18  ω     88.00 176.00   0.50    0.68    --  110.00  77.00 -60.00  176
 19  ω     95.00 149.00   0.50    0.68    --  110.00  57.00  60.00  108
 20  ω     98.00 126.00   0.50    0.68    --  110.00  38.00 150.00   56
 21  ω     98.00 145.00   0.50    0.68    --  110.00  38.00 120.00   94
 22  ω     94.00 134.00   0.50    0.68    --  110.00  57.00  30.00   80
 23  ω     86.00 114.00   0.50    0.68    --  110.00  77.00 120.00   56
 24  ω     86.00 171.00   0.50    0.68    --  110.00  77.00  90.00  170
 25  ω     86.00 112.00   0.50    0.68    --  110.00  77.00 150.00   52
 26  ω     86.00 116.00   0.50    0.68    --  110.00  77.00  60.00   60
 27  ω     86.00 114.00   0.50    0.68    --  110.00  77.00   0.00   56
 28  ω     86.00 112.00   0.50    0.68    --  110.00  77.00 -30.00   52
 29  ω     87.00 113.00   0.50    0.68    --  110.00  77.00  30.00   52
 30  ω     59.00  88.00   0.50    0.17    --   78.00  66.00  29.61   58
 31  ω     34.00 121.00   0.50    0.17    --   49.37  57.00 -60.00  174
 32  ω     62.00  98.00   0.50    0.68    --   86.00  79.00 -65.63   72
 33  ω     86.00 174.00   0.50    0.68    --  110.00  77.00-120.00  176
 34  ω     86.00 176.00   0.50    0.68    --  110.00  77.00-150.00  180
 35  ω     70.00  96.00   0.50    0.68    --  110.00 -99.00-120.00   52
 36  ω     61.00 102.00   0.50    0.68    --  110.00-125.00 -90.00   82
 37  ω     83.00 108.00   0.50    0.68    --  110.00 -99.00 -30.00   50
 38  ω     79.00 110.00   0.50    0.68    --  110.00 -99.00  60.00   62
 39  ω     79.00 110.00   0.50    0.68    --  110.00 -99.00 150.00   62
 40  ω     57.00 122.00   0.50    0.17    --   49.37-178.00 120.00  130
 41  ω     44.00  97.00   0.50    0.68    --  110.00 -99.00   0.00  106
 42  ω     48.00  76.00   0.50    0.68    --  110.00 -99.00 -30.00   56
 43  ω     45.00  92.00   0.50    0.68    --  110.00 -99.00 -60.00   94
 44  ω     41.00  90.00   0.50    0.68    --  110.00 -99.00-180.00   98
 45  ω     37.00 125.00   0.50    0.17    --   49.37  38.00 -60.00  176
 46  ω     34.00 121.00   0.50    0.17    --   49.37  57.00   0.00  174
 47  ω     34.00 121.00   0.50    0.17    --   49.37  57.00  30.00  174
 48  ω     37.00 125.00   0.50    0.17    --   49.37  38.00-120.00  176
 49  ω     30.00 120.00   0.50    0.17    --   54.00  79.00  44.96  180
 50  ω     25.00 116.00   0.50    0.17    --   50.00  80.00-107.59  182
 51  ω     29.00 120.00   0.50    0.17    --   54.00  80.00 -28.26  182
 52  ω     20.00  46.00   0.50    0.17    --   50.00  90.00 -73.30   52
 53  ω    -74.00  18.00   0.50    0.17    --  -38.00 102.00 129.21  184
 54  ω     28.00 121.00   0.50    0.17    --   54.00  82.00 165.28  186
 55  ω     45.00  75.00   0.50    0.68    --  110.00 -99.00  60.00   60
 56  ω     50.00  95.00   0.50    0.68    --  110.00 -99.00  90.00   90
 57  ω     46.00  73.00   0.50    0.68    --  110.00 -99.00 150.00   54
 58  ω    -93.00 -25.00   0.50    0.17    --  -26.00 156.00 175.55  136
 59  ω    -67.00   2.00   0.50    0.68    --  -70.00  57.00  30.00  138
 60  ω    -92.00 -24.00   0.50    0.17    --  -26.00 154.00 108.86  136
 61  ω   -125.00 -37.00   0.50    0.17    --  -49.87 -38.00 -90.00  176
 62  ω    -72.00 -44.00   0.50    0.68    --  -70.00 -82.00 -33.15   56
 63  ω    -71.00 -46.00   0.50    0.68    --  -70.00 -77.00 -90.00   50
 64  ω    -70.00 -43.00   0.50    0.68    --  -70.00 -83.00 -97.07   54
 65  ω    -76.00 -46.00   0.50    0.68    --  -70.00 -77.00   0.00   60
 66  ω    -72.00 -46.00   0.50    0.68    --  -70.00 -77.00  30.00   52
 67  ω    -77.00 -46.00   0.50    0.68    --  -70.00 -77.00  90.00   62
 68  ω    -81.00 -51.00   0.50    0.68    --  -70.00 -66.00 162.40   60
 69  ω    -92.00 -46.00   0.50    0.68    --  -70.00 -80.00 168.81   92
 70  ω    -85.00 -51.00   0.50    0.68    --  -70.00 -66.00  97.05   68
 71  ω    -96.00 -50.00   0.50    0.68    --  -70.00 -67.00 124.65   92
 72  ω   -133.00-102.00   0.50    0.68    --  -70.00 -66.00  97.05   62
 73  ω   -136.00 -46.00   0.50    0.68    --  -70.00 -77.00  60.00  180
 74  ω   -127.00-101.00   0.50    0.68    --  -70.00 -83.00 -97.07   52
 75  ω    -89.00 -47.00   0.50    0.68    --  -70.00 -75.00-159.21   84
 76  ω   -125.00 -37.00   0.50    0.17    --  -49.87 -38.00-180.00  176
 77  ω   -136.00 -47.00   0.50    0.68    --  -70.00 -74.00 -74.92  178
 78  ω   -136.00 -47.00   0.50    0.68    --  -70.00 -76.00-130.42  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 300K'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0064746000
_diffrn_orient_matrix_UB_12      -0.0009342000
_diffrn_orient_matrix_UB_13      0.0804840000
_diffrn_orient_matrix_UB_21      -0.0842810000
_diffrn_orient_matrix_UB_22      -0.0051905000
_diffrn_orient_matrix_UB_23      -0.0307914000
_diffrn_orient_matrix_UB_31      0.0024470000
_diffrn_orient_matrix_UB_32      -0.1844264000
_diffrn_orient_matrix_UB_33      0.0004909000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0173
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84976
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.771
_diffrn_reflns_theta_min         2.426
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.589
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.640
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.42a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_description       plank
_exptl_crystal_F_000             1180
_exptl_crystal_size_max          0.225
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.645
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     331
_refine_ls_number_reflns         6092
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0362
_refine_ls_R_factor_gt           0.0347
_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)+(0.0445P)²+2.4260P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.0933
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5761
_reflns_number_total             6092
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc02224a2.cif
_cod_data_source_block           ca230619_2_1
_cod_depositor_comments
;Adding full bibliography for 1557999.cif.

 Adding full bibliography for 1557999.cif.
;
_cod_database_code               1557999
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C28H30BrNO2Si
_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.
;
_diffrn_oxdiff_digest_frames
;
0189204a43a5b5c0d87bd6a43b39bdbed808198dade
;
_diffrn_oxdiff_digest_hkl
;
01c4f1d5028d6304c763d8cf878e0ea407a937
;
_reflns_odcompleteness_completeness 100.00
_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, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N1-H1
 0.93 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C8(H8)
3.b Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C2A(H2AA,
 H2AB), C3A(H3AA,H3AB)
3.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C19(H19), C20(H20), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28)
3.d Idealised Me refined as rotating group:
 C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C1A(H1AA,H1AB,H1AC)
;
_olex2_date_sample_data_collection 2019-06-28
_olex2_date_sample_submission    2019-06-27
_olex2_submission_original_sample_id ca230619_2_1
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.485
_oxdiff_exptl_absorpt_empirical_full_min 0.703
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Br1 Br 0.18321(2) 0.04918(3) 0.48636(2) 0.03955(8) Uani 1 1 d . . . . .
Si1 Si 0.70655(2) 0.18499(5) 0.77454(2) 0.02113(10) Uani 1 1 d . . . . .
O1 O 0.56227(7) 0.17497(16) 0.56728(7) 0.0304(3) Uani 1 1 d . . . . .
O2 O 0.60216(7) 0.40922(16) 0.62731(7) 0.0287(3) Uani 1 1 d . . . . .
N1 N 0.48341(8) 0.36391(18) 0.59009(8) 0.0259(3) Uani 1 1 d D . . . .
H1 H 0.4841(13) 0.454(2) 0.6155(12) 0.031 Uiso 1 1 d DR . . . .
C1 C 0.27806(10) 0.1451(2) 0.51890(10) 0.0266(3) Uani 1 1 d . . . . .
C2 C 0.29023(10) 0.2670(2) 0.57115(10) 0.0274(4) Uani 1 1 d . . . . .
H2 H 0.252768 0.301950 0.590341 0.033 Uiso 1 1 calc R . . . .
C3 C 0.33318(10) 0.0911(2) 0.49012(9) 0.0269(4) Uani 1 1 d . . . . .
H3 H 0.324046 0.008024 0.455502 0.032 Uiso 1 1 calc R . . . .
C4 C 0.35926(10) 0.3362(2) 0.59439(9) 0.0263(3) Uani 1 1 d . . . . .
H4 H 0.368316 0.417849 0.629737 0.032 Uiso 1 1 calc R . . . .
C5 C 0.40208(10) 0.1611(2) 0.51293(9) 0.0257(3) Uani 1 1 d . . . . .
H5 H 0.439207 0.125679 0.493362 0.031 Uiso 1 1 calc R . . . .
C6 C 0.41552(9) 0.2844(2) 0.56520(9) 0.0230(3) Uani 1 1 d . . . . .
C7 C 0.55041(9) 0.3033(2) 0.59206(9) 0.0243(3) Uani 1 1 d . . . . .
C8 C 0.67858(9) 0.3695(2) 0.63610(11) 0.0301(4) Uani 1 1 d . . . . .
H8 H 0.681993 0.266086 0.612482 0.036 Uiso 1 1 calc R . . . .
C9 C 0.72250(9) 0.3646(2) 0.71894(10) 0.0259(3) Uani 1 1 d . . . . .
C10 C 0.71417(12) 0.5000(3) 0.60100(14) 0.0480(6) Uani 1 1 d . . . . .
H10A H 0.700048 0.605824 0.613265 0.058 Uiso 1 1 calc R . . . .
H10B H 0.701284 0.488571 0.547053 0.058 Uiso 1 1 calc R . . . .
C11 C 0.71751(10) 0.5242(2) 0.76125(13) 0.0336(4) Uani 1 1 d . . . . .
H11A H 0.684993 0.602936 0.730515 0.040 Uiso 1 1 calc R . . . .
H11B H 0.705855 0.508227 0.808112 0.040 Uiso 1 1 calc R . . . .
C12 C 0.80378(10) 0.4164(3) 0.71879(13) 0.0359(4) Uani 1 1 d . . . . .
C13 C 0.79607(12) 0.4694(3) 0.63698(15) 0.0519(7) Uani 1 1 d . . . . .
H13A H 0.824157 0.566162 0.636365 0.062 Uiso 1 1 calc R . . . .
H13B H 0.813663 0.386032 0.610230 0.062 Uiso 1 1 calc R . . . .
C14 C 0.61554(9) 0.21179(19) 0.79523(9) 0.0213(3) Uani 1 1 d . . . . .
C15 C 0.70084(10) -0.0103(2) 0.72376(11) 0.0294(4) Uani 1 1 d . . . . .
H15A H 0.686789 -0.093461 0.752448 0.044 Uiso 1 1 calc GR . . . .
H15B H 0.747846 -0.035206 0.716976 0.044 Uiso 1 1 calc GR . . . .
H15C H 0.664952 -0.002201 0.675820 0.044 Uiso 1 1 calc GR . . . .
C16 C 0.77941(10) 0.1746(2) 0.86655(10) 0.0315(4) Uani 1 1 d . . . . .
H16A H 0.790031 0.280600 0.886672 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.823113 0.128155 0.859357 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.762396 0.109789 0.900742 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.79953(12) 0.5579(3) 0.77118(16) 0.0464(6) Uani 1 1 d . . . . .
H17A H 0.830126 0.543409 0.822126 0.056 Uiso 1 1 calc R . . . .
H17B H 0.808593 0.661348 0.751870 0.056 Uiso 1 1 calc R . . . .
C18 C 0.86622(10) 0.2981(3) 0.74490(12) 0.0372(5) Uani 1 1 d . . . . .
C19 C 0.55089(9) 0.1439(2) 0.74935(9) 0.0224(3) Uani 1 1 d . . . . .
H19 H 0.552358 0.089996 0.706179 0.027 Uiso 1 1 calc R . . . .
C20 C 0.61077(10) 0.2912(2) 0.85993(10) 0.0259(3) Uani 1 1 d . . . . .
H20 H 0.652783 0.337046 0.891682 0.031 Uiso 1 1 calc R . . . .
C21 C 0.86330(12) 0.1523(3) 0.70765(12) 0.0412(5) Uani 1 1 d . . . . .
H21 H 0.823362 0.130229 0.666606 0.049 Uiso 1 1 calc R . . . .
C22 C 0.92774(11) 0.3291(3) 0.80467(14) 0.0455(5) Uani 1 1 d . . . . .
H22 H 0.931560 0.425799 0.830205 0.055 Uiso 1 1 calc R . . . .
C23 C 0.48450(9) 0.1552(2) 0.76674(10) 0.0252(3) Uani 1 1 d . . . . .
H23 H 0.442294 0.109469 0.735320 0.030 Uiso 1 1 calc R . . . .
C24 C 0.54457(10) 0.3032(2) 0.87776(10) 0.0276(4) Uani 1 1 d . . . . .
H24 H 0.542698 0.356833 0.920875 0.033 Uiso 1 1 calc R . . . .
C25 C 0.91882(14) 0.0393(3) 0.73064(15) 0.0512(6) Uani 1 1 d . . . . .
H25 H 0.915157 -0.058297 0.705847 0.061 Uiso 1 1 calc R . . . .
C26 C 0.98396(11) 0.2155(4) 0.82663(15) 0.0521(7) Uani 1 1 d . . . . .
H26 H 1.024976 0.237829 0.866488 0.062 Uiso 1 1 calc R . . . .
C27 C 0.48150(10) 0.2350(2) 0.83120(10) 0.0266(3) Uani 1 1 d . . . . .
H27 H 0.437279 0.242665 0.843062 0.032 Uiso 1 1 calc R . . . .
C28 C 0.97928(13) 0.0716(3) 0.79008(15) 0.0523(7) Uani 1 1 d . . . . .
H28 H 1.016671 -0.003593 0.805326 0.063 Uiso 1 1 calc R . . . .
C1A C 0.99573(19) 0.6672(5) 0.9217(2) 0.0837(10) Uani 1 1 d . . . . .
H1AA H 0.971517 0.705633 0.872360 0.126 Uiso 1 1 calc GR . . . .
H1AB H 0.960085 0.622162 0.943501 0.126 Uiso 1 1 calc GR . . . .
H1AC H 1.030874 0.586583 0.918966 0.126 Uiso 1 1 calc GR . . . .
C2A C 1.03398(16) 0.8022(5) 0.96877(18) 0.0770(10) Uani 1 1 d . . . . .
H2AA H 1.069014 0.849008 0.945856 0.092 Uiso 1 1 calc R . . . .
H2AB H 1.061081 0.761464 1.017528 0.092 Uiso 1 1 calc R . . . .
C3A C 0.98129(16) 0.9310(5) 0.97865(16) 0.0738(10) Uani 1 1 d . . . . .
H3AA H 0.952156 0.966987 0.929758 0.089 Uiso 1 1 calc R . . . .
H3AB H 0.948054 0.885346 1.004136 0.089 Uiso 1 1 calc R . . . .
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'
Br Br -0.6763 1.2805 '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
-1 0 0 0.0270
1 0 0 0.0153
0 -1 0 0.1108
-1 2 0 0.1073
0 0 1 0.0387
0 0 -1 0.0315
10 -3 -5 0.0709
7 4 -4 0.1042
4 0 10 0.0333
3 -2 10 0.0478
-7 0 11 0.0432
11 2 2 0.0459
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
C14 Si1 C9 108.43(7) . . ?
C15 Si1 C9 114.03(8) . . ?
C15 Si1 C14 106.36(8) . . ?
C15 Si1 C16 110.12(9) . . ?
C16 Si1 C9 110.22(8) . . ?
C16 Si1 C14 107.38(8) . . ?
C7 O2 C8 118.21(14) . . ?
C6 N1 H1 116.7(15) . . ?
C7 N1 H1 115.4(15) . . ?
C7 N1 C6 126.59(15) . . ?
C2 C1 Br1 119.14(14) . . ?
C3 C1 Br1 119.46(14) . . ?
C3 C1 C2 121.41(17) . . ?
C1 C2 H2 120.6 . . ?
C1 C2 C4 118.74(16) . . ?
C4 C2 H2 120.6 . . ?
C1 C3 H3 120.1 . . ?
C1 C3 C5 119.87(16) . . ?
C5 C3 H3 120.1 . . ?
C2 C4 H4 119.7 . . ?
C2 C4 C6 120.66(16) . . ?
C6 C4 H4 119.7 . . ?
C3 C5 H5 120.1 . . ?
C3 C5 C6 119.75(16) . . ?
C6 C5 H5 120.1 . . ?
C4 C6 N1 117.13(15) . . ?
C5 C6 N1 123.29(15) . . ?
C5 C6 C4 119.57(16) . . ?
O1 C7 O2 125.25(16) . . ?
O1 C7 N1 126.30(17) . . ?
O2 C7 N1 108.44(15) . . ?
O2 C8 H8 110.0 . . ?
O2 C8 C9 111.07(14) . . ?
O2 C8 C10 109.87(15) . . ?
C9 C8 H8 110.0 . . ?
C10 C8 H8 110.0 . . ?
C10 C8 C9 105.74(17) . . ?
C8 C9 Si1 116.52(13) . . ?
C8 C9 C11 113.03(15) . . ?
C8 C9 C12 103.81(14) . . ?
C11 C9 Si1 110.84(13) . . ?
C11 C9 C12 88.14(14) . . ?
C12 C9 Si1 121.22(12) . . ?
C8 C10 H10A 111.3 . . ?
C8 C10 H10B 111.3 . . ?
C8 C10 C13 102.28(16) . . ?
H10A C10 H10B 109.2 . . ?
C13 C10 H10A 111.3 . . ?
C13 C10 H10B 111.3 . . ?
C9 C11 H11A 113.5 . . ?
C9 C11 H11B 113.5 . . ?
H11A C11 H11B 110.8 . . ?
C17 C11 C9 90.67(15) . . ?
C17 C11 H11A 113.5 . . ?
C17 C11 H11B 113.5 . . ?
C13 C12 C9 104.88(16) . . ?
C17 C12 C9 88.95(15) . . ?
C17 C12 C13 113.22(19) . . ?
C18 C12 C9 119.33(16) . . ?
C18 C12 C13 110.34(18) . . ?
C18 C12 C17 118.13(19) . . ?
C10 C13 C12 106.12(17) . . ?
C10 C13 H13A 110.5 . . ?
C10 C13 H13B 110.5 . . ?
C12 C13 H13A 110.5 . . ?
C12 C13 H13B 110.5 . . ?
H13A C13 H13B 108.7 . . ?
C19 C14 Si1 121.45(12) . . ?
C19 C14 C20 117.15(15) . . ?
C20 C14 Si1 121.26(13) . . ?
Si1 C15 H15A 109.5 . . ?
Si1 C15 H15B 109.5 . . ?
Si1 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Si1 C16 H16A 109.5 . . ?
Si1 C16 H16B 109.5 . . ?
Si1 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 C12 91.00(16) . . ?
C11 C17 H17A 113.5 . . ?
C11 C17 H17B 113.5 . . ?
C12 C17 H17A 113.5 . . ?
C12 C17 H17B 113.5 . . ?
H17A C17 H17B 110.8 . . ?
C21 C18 C12 119.54(19) . . ?
C22 C18 C12 122.6(2) . . ?
C22 C18 C21 117.8(2) . . ?
C14 C19 H19 119.2 . . ?
C23 C19 C14 121.70(15) . . ?
C23 C19 H19 119.2 . . ?
C14 C20 H20 119.2 . . ?
C24 C20 C14 121.54(16) . . ?
C24 C20 H20 119.2 . . ?
C18 C21 H21 119.3 . . ?
C25 C21 C18 121.3(2) . . ?
C25 C21 H21 119.3 . . ?
C18 C22 H22 119.8 . . ?
C18 C22 C26 120.4(3) . . ?
C26 C22 H22 119.8 . . ?
C19 C23 H23 120.1 . . ?
C27 C23 C19 119.81(16) . . ?
C27 C23 H23 120.1 . . ?
C20 C24 H24 120.0 . . ?
C27 C24 C20 119.96(16) . . ?
C27 C24 H24 120.0 . . ?
C21 C25 H25 119.9 . . ?
C28 C25 C21 120.1(3) . . ?
C28 C25 H25 119.9 . . ?
C22 C26 H26 119.6 . . ?
C28 C26 C22 120.8(2) . . ?
C28 C26 H26 119.6 . . ?
C23 C27 H27 120.1 . . ?
C24 C27 C23 119.84(16) . . ?
C24 C27 H27 120.1 . . ?
C25 C28 H28 120.2 . . ?
C26 C28 C25 119.5(2) . . ?
C26 C28 H28 120.2 . . ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
C2A C1A H1AA 109.5 . . ?
C2A C1A H1AB 109.5 . . ?
C2A C1A H1AC 109.5 . . ?
C1A C2A H2AA 109.1 . . ?
C1A C2A H2AB 109.1 . . ?
C1A C2A C3A 112.4(3) . . ?
H2AA C2A H2AB 107.9 . . ?
C3A C2A H2AA 109.1 . . ?
C3A C2A H2AB 109.1 . . ?
C2A C3A H3AA 109.0 . . ?
C2A C3A H3AB 109.0 . . ?
C3A C3A C2A 112.9(3) 3_777 . ?
C3A C3A H3AA 109.0 3_777 . ?
C3A C3A H3AB 109.0 3_777 . ?
H3AA C3A H3AB 107.8 . . ?
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
Br1 C1 1.9067(18) . ?
Si1 C9 1.8959(18) . ?
Si1 C14 1.8893(17) . ?
Si1 C15 1.8732(19) . ?
Si1 C16 1.8751(19) . ?
O1 C7 1.213(2) . ?
O2 C7 1.347(2) . ?
O2 C8 1.453(2) . ?
N1 H1 0.890(16) . ?
N1 C6 1.407(2) . ?
N1 C7 1.361(2) . ?
C1 C2 1.382(3) . ?
C1 C3 1.381(3) . ?
C2 H2 0.9300 . ?
C2 C4 1.385(3) . ?
C3 H3 0.9300 . ?
C3 C5 1.385(3) . ?
C4 H4 0.9300 . ?
C4 C6 1.399(2) . ?
C5 H5 0.9300 . ?
C5 C6 1.391(2) . ?
C8 H8 0.9800 . ?
C8 C9 1.533(3) . ?
C8 C10 1.525(3) . ?
C9 C11 1.566(3) . ?
C9 C12 1.605(2) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C13 1.530(3) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 C17 1.542(3) . ?
C12 C13 1.555(3) . ?
C12 C17 1.550(3) . ?
C12 C18 1.514(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C14 C19 1.401(2) . ?
C14 C20 1.403(2) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C21 1.395(3) . ?
C18 C22 1.391(3) . ?
C19 H19 0.9300 . ?
C19 C23 1.392(2) . ?
C20 H20 0.9300 . ?
C20 C24 1.393(2) . ?
C21 H21 0.9300 . ?
C21 C25 1.389(3) . ?
C22 H22 0.9300 . ?
C22 C26 1.400(3) . ?
C23 H23 0.9300 . ?
C23 C27 1.390(3) . ?
C24 H24 0.9300 . ?
C24 C27 1.386(3) . ?
C25 H25 0.9300 . ?
C25 C28 1.377(4) . ?
C26 H26 0.9300 . ?
C26 C28 1.372(4) . ?
C27 H27 0.9300 . ?
C28 H28 0.9300 . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C1A C2A 1.485(5) . ?
C2A H2AA 0.9700 . ?
C2A H2AB 0.9700 . ?
C2A C3A 1.516(5) . ?
C3A C3A 1.465(8) 3_777 ?
C3A H3AA 0.9700 . ?
C3A H3AB 0.9700 . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 168306357
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
-1.0001 0.0002 0.0002 0.0065 0.0843 -0.0025
1.0001 -0.0002 -0.0002 -0.0065 -0.0843 0.0025
-0.0001 -1.0001 0.0019 0.0011 0.0051 0.1844
-0.9998 2.0003 -0.0035 0.0043 0.0740 -0.3714
0.0002 0.0002 0.9998 0.0805 -0.0308 0.0005
-0.0002 -0.0002 -0.9998 -0.0805 0.0308 -0.0005
9.7383 -3.0896 -5.3577 -0.4914 -0.6397 0.5910
6.8592 4.4055 -3.9405 -0.3657 -0.4796 -0.7976
3.5073 0.0244 10.1452 0.7938 -0.6081 0.0091
3.4594 -1.5053 9.6939 0.7592 -0.5822 0.2908
-7.4910 -0.2313 11.2999 0.9582 0.2846 0.0299
10.6352 1.5882 1.8290 0.0769 -0.9609 -0.2660
