#------------------------------------------------------------------------------
#$Date: 2024-07-05 17:08:42 +0200 (Fri 05 de Jul de 2024) $
#$Revision: 292929 $
#$URL: svn://www.crystallography.net/cod/cif/1/57/15/1571513.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_1571513
loop_
_publ_author_name
'Chinta, Bhavani Shankar'
'Sneddon, Dorian S.'
'Hoye, Thomas R.'
_publ_section_title
;
 Cascade reactions of HDDA-benzynes with tethered cyclohexadienones:
 strain-driven events originating from ortho-annulated
 benzocyclobutenes.
;
_journal_issue                   21
_journal_name_full               'Chemical science'
_journal_page_first              8181
_journal_page_last               8189
_journal_paper_doi               10.1039/d4sc00571f
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'C32 H42 N2 O9 Os Si'
_chemical_formula_sum            'C32 H42 N2 O9 Os Si'
_chemical_formula_weight         816.96
_chemical_name_common            21159z
_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   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-10-21 deposited with the CCDC.	2024-04-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.919(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5341(6)
_cell_length_b                   19.6037(12)
_cell_length_c                   13.2334(6)
_cell_measurement_reflns_used    2880
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.45
_cell_measurement_theta_min      2.50
_cell_volume                     3249.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker PHOTON-III CPAD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_unetI/netI     0.0488
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34620
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.526
_diffrn_reflns_theta_min         1.929
_diffrn_source                   micro-focus
_exptl_absorpt_coefficient_mu    4.017
_exptl_absorpt_correction_T_max  0.4330
_exptl_absorpt_correction_T_min  0.3496
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS-2016/1, Sheldrick'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.670
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_transmission_factor_max   0.4330
_exptl_transmission_factor_min   0.3496
_refine_diff_density_max         1.360
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         9901
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0289
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0223P)²+1.1279P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7706
_reflns_number_total             9901
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4sc00571f2.cif
_cod_data_source_block           21159z
_cod_depositor_comments
'Adding full bibliography for 1571511--1571514.cif.'
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1571513
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.666
_shelx_estimated_absorpt_t_max   0.961
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
Os1 Os 0.73027(2) 0.07285(2) 0.41453(2) 0.01628(3) Uani 1 1 d . . . . .
Si1 Si 0.91665(6) 0.21694(5) 0.22752(6) 0.02092(17) Uani 1 1 d . . . . .
O1 O 0.76986(18) 0.58089(11) 0.52860(17) 0.0308(5) Uani 1 1 d . . . . .
N1 N 0.80773(19) -0.02667(13) 0.36999(18) 0.0224(5) Uani 1 1 d . . . . .
C1 C 0.8622(3) 0.61411(18) 0.4928(3) 0.0368(8) Uani 1 1 d . . . . .
H1 H 0.861810 0.662067 0.513705 0.055 Uiso 1 1 calc R U . . .
H2 H 0.862036 0.611434 0.418853 0.055 Uiso 1 1 calc R U . . .
H3 H 0.926353 0.591715 0.521213 0.055 Uiso 1 1 calc R U . . .
O2 O 0.60513(17) 0.52614(11) 0.60041(15) 0.0245(5) Uani 1 1 d . . . . .
N2 N 0.73955(19) 0.02330(14) 0.56538(17) 0.0215(5) Uani 1 1 d . . . . .
C2 C 0.5276(2) 0.49355(16) 0.6617(2) 0.0232(6) Uani 1 1 d . . . . .
H4 H 0.500169 0.526575 0.710053 0.035 Uiso 1 1 calc R U . . .
H5 H 0.561111 0.455399 0.698607 0.035 Uiso 1 1 calc R U . . .
H6 H 0.468526 0.476461 0.618408 0.035 Uiso 1 1 calc R U . . .
O3 O 0.94178(16) 0.36231(12) 0.33314(16) 0.0293(5) Uani 1 1 d . . . . .
C3 C 0.7541(2) 0.51487(15) 0.4999(2) 0.0213(6) Uani 1 1 d . . . . .
O4 O 0.52996(15) 0.18162(11) 0.18047(13) 0.0189(4) Uani 1 1 d . . . . .
C4 C 0.6608(2) 0.48498(15) 0.5381(2) 0.0206(6) Uani 1 1 d . . . . .
O5 O 0.38006(17) 0.18171(11) 0.50010(15) 0.0268(5) Uani 1 1 d . . . . .
C5 C 0.8208(2) 0.47659(16) 0.4402(2) 0.0218(6) Uani 1 1 d . . . . .
H7 H 0.885060 0.495356 0.416093 0.026 Uiso 1 1 calc R U . . .
O6 O 0.66386(14) 0.15586(10) 0.46376(13) 0.0169(4) Uani 1 1 d . . . . .
C6 C 0.6301(2) 0.41979(14) 0.5118(2) 0.0179(6) Uani 1 1 d . . . . .
H8 H 0.566230 0.400760 0.536208 0.022 Uiso 1 1 calc R U . . .
O7 O 0.71793(15) 0.11928(10) 0.28270(13) 0.0168(4) Uani 1 1 d . . . . .
C7 C 0.7907(2) 0.40989(15) 0.4166(2) 0.0199(6) Uani 1 1 d . . . . .
O8 O 0.61314(15) 0.02523(11) 0.40088(15) 0.0229(4) Uani 1 1 d . . . . .
C8 C 0.6951(2) 0.38202(15) 0.44832(19) 0.0169(5) Uani 1 1 d . . . . .
O9 O 0.86348(15) 0.09470(11) 0.44042(15) 0.0214(4) Uani 1 1 d . . . . .
C9 C 0.8519(2) 0.35642(16) 0.3644(2) 0.0199(6) Uani 1 1 d . . . . .
C10 C 0.7810(2) 0.29411(15) 0.35744(19) 0.0169(6) Uani 1 1 d . . . . .
C11 C 0.6832(2) 0.31209(15) 0.41302(19) 0.0163(5) Uani 1 1 d . . . . .
C12 C 0.7914(2) 0.23683(15) 0.30163(19) 0.0165(5) Uani 1 1 d . . . . .
C13 C 0.6033(2) 0.26756(15) 0.41926(19) 0.0162(5) Uani 1 1 d . . . . .
C14 C 0.6914(2) 0.19021(15) 0.29175(19) 0.0162(5) Uani 1 1 d . . . . .
C15 C 0.6184(2) 0.19597(14) 0.38112(19) 0.0152(5) Uani 1 1 d . . . . .
C16 C 0.6313(2) 0.21368(15) 0.19541(19) 0.0178(5) Uani 1 1 d . . . . .
H18 H 0.620858 0.263681 0.198590 0.021 Uiso 1 1 calc R U . . .
H19 H 0.675474 0.203830 0.136522 0.021 Uiso 1 1 calc R U . . .
C17 C 0.4549(2) 0.19646(15) 0.2583(2) 0.0180(6) Uani 1 1 d . . . . .
C18 C 0.5028(2) 0.17005(14) 0.35995(19) 0.0155(5) Uani 1 1 d . . . . .
H23 H 0.498094 0.119258 0.365109 0.019 Uiso 1 1 calc R U . . .
C19 C 0.4458(2) 0.20529(15) 0.4452(2) 0.0182(6) Uani 1 1 d . . . . .
C20 C 0.4868(2) 0.27805(15) 0.4436(2) 0.0182(6) Uani 1 1 d . . . . .
H24 H 0.474834 0.304736 0.506586 0.022 Uiso 1 1 calc R U . . .
C21 C 0.4347(2) 0.30811(15) 0.3475(2) 0.0204(6) Uani 1 1 d . . . . .
H25 H 0.407777 0.353389 0.347994 0.024 Uiso 1 1 calc R U . . .
C22 C 0.4269(2) 0.27104(15) 0.2627(2) 0.0201(6) Uani 1 1 d . . . . .
H26 H 0.402350 0.292890 0.202230 0.024 Uiso 1 1 calc R U . . .
C23 C 0.9010(3) 0.13711(19) 0.1507(3) 0.0356(8) Uani 1 1 d . . . . .
H9 H 0.948126 0.139082 0.093230 0.053 Uiso 1 1 calc R U . . .
H10 H 0.826720 0.132923 0.125890 0.053 Uiso 1 1 calc R U . . .
H11 H 0.919837 0.097545 0.192936 0.053 Uiso 1 1 calc R U . . .
C24 C 0.9465(3) 0.28262(19) 0.1304(3) 0.0410(9) Uani 1 1 d . . . . .
H12 H 1.009079 0.268445 0.093103 0.061 Uiso 1 1 calc R U . . .
H13 H 0.961254 0.326419 0.163690 0.061 Uiso 1 1 calc R U . . .
H14 H 0.885008 0.287480 0.083249 0.061 Uiso 1 1 calc R U . . .
C25 C 1.0310(3) 0.2050(2) 0.3196(3) 0.0381(9) Uani 1 1 d . . . . .
H15 H 1.094643 0.191781 0.283305 0.057 Uiso 1 1 calc R U . . .
H16 H 1.013548 0.169126 0.367940 0.057 Uiso 1 1 calc R U . . .
H17 H 1.044838 0.247791 0.356003 0.057 Uiso 1 1 calc R U . . .
C26 C 0.3549(2) 0.15657(16) 0.2270(2) 0.0228(6) Uani 1 1 d . . . . .
H20 H 0.301370 0.161704 0.278731 0.034 Uiso 1 1 calc R U . . .
H21 H 0.372884 0.108211 0.219663 0.034 Uiso 1 1 calc R U . . .
H22 H 0.326082 0.174145 0.162308 0.034 Uiso 1 1 calc R U . . .
C27 C 0.8520(3) -0.05448(18) 0.4680(2) 0.0312(7) Uani 1 1 d . . . . .
H33 H 0.917256 -0.028927 0.488582 0.037 Uiso 1 1 calc R U . . .
H34 H 0.871794 -0.102931 0.459047 0.037 Uiso 1 1 calc R U . . .
C28 C 0.7720(3) -0.04890(17) 0.5492(2) 0.0285(7) Uani 1 1 d . . . . .
H35 H 0.708170 -0.076367 0.530085 0.034 Uiso 1 1 calc R U . . .
H36 H 0.803137 -0.067632 0.613099 0.034 Uiso 1 1 calc R U . . .
C29 C 0.8963(3) -0.0176(2) 0.3004(3) 0.0356(8) Uani 1 1 d . . . . .
H27 H 0.931276 -0.061616 0.289738 0.053 Uiso 1 1 calc R U . . .
H28 H 0.948210 0.014765 0.329834 0.053 Uiso 1 1 calc R U . . .
H29 H 0.868247 0.000033 0.235545 0.053 Uiso 1 1 calc R U . . .
C30 C 0.7330(3) -0.07726(17) 0.3225(3) 0.0320(7) Uani 1 1 d . . . . .
H30 H 0.770976 -0.120174 0.311435 0.048 Uiso 1 1 calc R U . . .
H31 H 0.705257 -0.059513 0.257592 0.048 Uiso 1 1 calc R U . . .
H32 H 0.673607 -0.085400 0.367296 0.048 Uiso 1 1 calc R U . . .
C31 C 0.8162(3) 0.05805(17) 0.6346(2) 0.0298(7) Uani 1 1 d . . . . .
H40 H 0.816467 0.035771 0.700905 0.045 Uiso 1 1 calc R U . . .
H41 H 0.795423 0.105952 0.641766 0.045 Uiso 1 1 calc R U . . .
H42 H 0.887795 0.055555 0.607217 0.045 Uiso 1 1 calc R U . . .
C32 C 0.6340(3) 0.0254(2) 0.6133(3) 0.0379(9) Uani 1 1 d . . . . .
H37 H 0.640438 0.005456 0.681148 0.057 Uiso 1 1 calc R U . . .
H38 H 0.582022 -0.000728 0.572138 0.057 Uiso 1 1 calc R U . . .
H39 H 0.610107 0.072831 0.618234 0.057 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 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.6030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Os1 O9 161.35(10) . . ?
O8 Os1 O6 96.55(9) . . ?
O9 Os1 O6 98.38(9) . . ?
O8 Os1 O7 96.59(9) . . ?
O9 Os1 O7 96.12(8) . . ?
O6 Os1 O7 83.59(8) . . ?
O8 Os1 N2 82.96(9) . . ?
O9 Os1 N2 84.83(9) . . ?
O6 Os1 N2 94.29(8) . . ?
O7 Os1 N2 177.79(8) . . ?
O8 Os1 N1 83.03(9) . . ?
O9 Os1 N1 81.20(9) . . ?
O6 Os1 N1 175.50(8) . . ?
O7 Os1 N1 100.90(8) . . ?
N2 Os1 N1 81.21(9) . . ?
C25 Si1 C24 111.67(18) . . ?
C25 Si1 C23 108.31(17) . . ?
C24 Si1 C23 102.86(16) . . ?
C25 Si1 C12 108.39(13) . . ?
C24 Si1 C12 113.48(14) . . ?
C23 Si1 C12 111.99(13) . . ?
C3 O1 C1 117.0(2) . . ?
C29 N1 C30 107.0(3) . . ?
C29 N1 C27 108.7(2) . . ?
C30 N1 C27 109.4(3) . . ?
C29 N1 Os1 113.3(2) . . ?
C30 N1 Os1 114.48(19) . . ?
C27 N1 Os1 103.75(18) . . ?
O1 C1 H1 109.5 . . ?
O1 C1 H2 109.5 . . ?
H1 C1 H2 109.5 . . ?
O1 C1 H3 109.5 . . ?
H1 C1 H3 109.5 . . ?
H2 C1 H3 109.5 . . ?
C4 O2 C2 116.6(2) . . ?
C31 N2 C32 107.1(3) . . ?
C31 N2 C28 110.7(3) . . ?
C32 N2 C28 109.8(3) . . ?
C31 N2 Os1 111.75(18) . . ?
C32 N2 Os1 110.56(19) . . ?
C28 N2 Os1 107.03(17) . . ?
O2 C2 H4 109.5 . . ?
O2 C2 H5 109.5 . . ?
H4 C2 H5 109.5 . . ?
O2 C2 H6 109.5 . . ?
H4 C2 H6 109.5 . . ?
H5 C2 H6 109.5 . . ?
O1 C3 C5 126.0(3) . . ?
O1 C3 C4 114.1(2) . . ?
C5 C3 C4 120.0(3) . . ?
C16 O4 C17 114.2(2) . . ?
O2 C4 C6 124.0(3) . . ?
O2 C4 C3 114.6(3) . . ?
C6 C4 C3 121.4(3) . . ?
C3 C5 C7 118.1(3) . . ?
C3 C5 H7 121.0 . . ?
C7 C5 H7 121.0 . . ?
C15 O6 Os1 111.25(14) . . ?
C4 C6 C8 118.7(2) . . ?
C4 C6 H8 120.7 . . ?
C8 C6 H8 120.7 . . ?
C14 O7 Os1 112.67(15) . . ?
C5 C7 C8 122.0(3) . . ?
C5 C7 C9 128.8(3) . . ?
C8 C7 C9 109.0(2) . . ?
C7 C8 C6 119.7(3) . . ?
C7 C8 C11 110.6(2) . . ?
C6 C8 C11 129.5(2) . . ?
O3 C9 C7 126.1(3) . . ?
O3 C9 C10 127.2(3) . . ?
C7 C9 C10 106.7(2) . . ?
C12 C10 C11 124.1(3) . . ?
C12 C10 C9 129.6(2) . . ?
C11 C10 C9 105.7(2) . . ?
C13 C11 C8 131.8(3) . . ?
C13 C11 C10 120.5(3) . . ?
C8 C11 C10 107.7(2) . . ?
C10 C12 C14 116.3(2) . . ?
C10 C12 Si1 122.9(2) . . ?
C14 C12 Si1 120.60(19) . . ?
C11 C13 C15 119.1(2) . . ?
C11 C13 C20 130.8(3) . . ?
C15 C13 C20 109.3(2) . . ?
O7 C14 C15 106.5(2) . . ?
O7 C14 C16 109.3(2) . . ?
C15 C14 C16 109.4(2) . . ?
O7 C14 C12 112.9(2) . . ?
C15 C14 C12 113.3(2) . . ?
C16 C14 C12 105.5(2) . . ?
O6 C15 C13 107.7(2) . . ?
O6 C15 C14 108.4(2) . . ?
C13 C15 C14 114.5(2) . . ?
O6 C15 C18 107.4(2) . . ?
C13 C15 C18 103.8(2) . . ?
C14 C15 C18 114.6(2) . . ?
O4 C16 C14 113.3(2) . . ?
O4 C16 H18 108.9 . . ?
C14 C16 H18 108.9 . . ?
O4 C16 H19 108.9 . . ?
C14 C16 H19 108.9 . . ?
H18 C16 H19 107.7 . . ?
O4 C17 C22 112.4(2) . . ?
O4 C17 C26 104.6(2) . . ?
C22 C17 C26 108.5(2) . . ?
O4 C17 C18 108.0(2) . . ?
C22 C17 C18 112.1(2) . . ?
C26 C17 C18 111.0(2) . . ?
C19 C18 C17 108.4(2) . . ?
C19 C18 C15 100.2(2) . . ?
C17 C18 C15 112.4(2) . . ?
C19 C18 H23 111.8 . . ?
C17 C18 H23 111.8 . . ?
C15 C18 H23 111.8 . . ?
O5 C19 C20 127.3(3) . . ?
O5 C19 C18 128.2(3) . . ?
C20 C19 C18 104.4(2) . . ?
C19 C20 C13 101.8(2) . . ?
C19 C20 C21 103.8(2) . . ?
C13 C20 C21 105.2(2) . . ?
C19 C20 H24 114.8 . . ?
C13 C20 H24 114.8 . . ?
C21 C20 H24 114.8 . . ?
C22 C21 C20 120.4(3) . . ?
C22 C21 H25 119.8 . . ?
C20 C21 H25 119.8 . . ?
C21 C22 C17 123.3(3) . . ?
C21 C22 H26 118.3 . . ?
C17 C22 H26 118.3 . . ?
Si1 C23 H9 109.5 . . ?
Si1 C23 H10 109.5 . . ?
H9 C23 H10 109.5 . . ?
Si1 C23 H11 109.5 . . ?
H9 C23 H11 109.5 . . ?
H10 C23 H11 109.5 . . ?
Si1 C24 H12 109.5 . . ?
Si1 C24 H13 109.5 . . ?
H12 C24 H13 109.5 . . ?
Si1 C24 H14 109.5 . . ?
H12 C24 H14 109.5 . . ?
H13 C24 H14 109.5 . . ?
Si1 C25 H15 109.5 . . ?
Si1 C25 H16 109.5 . . ?
H15 C25 H16 109.5 . . ?
Si1 C25 H17 109.5 . . ?
H15 C25 H17 109.5 . . ?
H16 C25 H17 109.5 . . ?
C17 C26 H20 109.5 . . ?
C17 C26 H21 109.5 . . ?
H20 C26 H21 109.5 . . ?
C17 C26 H22 109.5 . . ?
H20 C26 H22 109.5 . . ?
H21 C26 H22 109.5 . . ?
N1 C27 C28 111.0(3) . . ?
N1 C27 H33 109.4 . . ?
C28 C27 H33 109.4 . . ?
N1 C27 H34 109.4 . . ?
C28 C27 H34 109.4 . . ?
H33 C27 H34 108.0 . . ?
N2 C28 C27 111.4(3) . . ?
N2 C28 H35 109.3 . . ?
C27 C28 H35 109.3 . . ?
N2 C28 H36 109.3 . . ?
C27 C28 H36 109.3 . . ?
H35 C28 H36 108.0 . . ?
N1 C29 H27 109.5 . . ?
N1 C29 H28 109.5 . . ?
H27 C29 H28 109.5 . . ?
N1 C29 H29 109.5 . . ?
H27 C29 H29 109.5 . . ?
H28 C29 H29 109.5 . . ?
N1 C30 H30 109.5 . . ?
N1 C30 H31 109.5 . . ?
H30 C30 H31 109.5 . . ?
N1 C30 H32 109.5 . . ?
H30 C30 H32 109.5 . . ?
H31 C30 H32 109.5 . . ?
N2 C31 H40 109.5 . . ?
N2 C31 H41 109.5 . . ?
H40 C31 H41 109.5 . . ?
N2 C31 H42 109.5 . . ?
H40 C31 H42 109.5 . . ?
H41 C31 H42 109.5 . . ?
N2 C32 H37 109.5 . . ?
N2 C32 H38 109.5 . . ?
H37 C32 H38 109.5 . . ?
N2 C32 H39 109.5 . . ?
H37 C32 H39 109.5 . . ?
H38 C32 H39 109.5 . . ?
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
Os1 O8 1.744(2) . ?
Os1 O9 1.747(2) . ?
Os1 O6 1.9498(19) . ?
Os1 O7 1.9692(18) . ?
Os1 N2 2.219(2) . ?
Os1 N1 2.266(3) . ?
Si1 C25 1.865(4) . ?
Si1 C24 1.867(3) . ?
Si1 C23 1.873(3) . ?
Si1 C12 1.919(3) . ?
O1 C3 1.361(3) . ?
O1 C1 1.423(4) . ?
N1 C29 1.477(4) . ?
N1 C30 1.489(4) . ?
N1 C27 1.496(4) . ?
C1 H1 0.9800 . ?
C1 H2 0.9800 . ?
C1 H3 0.9800 . ?
O2 C4 1.362(3) . ?
O2 C2 1.437(3) . ?
N2 C31 1.472(4) . ?
N2 C32 1.486(4) . ?
N2 C28 1.490(4) . ?
C2 H4 0.9800 . ?
C2 H5 0.9800 . ?
C2 H6 0.9800 . ?
O3 C9 1.219(3) . ?
C3 C5 1.390(4) . ?
C3 C4 1.417(4) . ?
O4 C16 1.425(3) . ?
O4 C17 1.447(3) . ?
C4 C6 1.376(4) . ?
O5 C19 1.209(3) . ?
C5 C7 1.393(4) . ?
C5 H7 0.9500 . ?
O6 C15 1.448(3) . ?
C6 C8 1.401(4) . ?
C6 H8 0.9500 . ?
O7 C14 1.436(3) . ?
C7 C8 1.394(4) . ?
C7 C9 1.483(4) . ?
C8 C11 1.454(4) . ?
C9 C10 1.511(4) . ?
C10 C12 1.353(4) . ?
C10 C11 1.493(3) . ?
C11 C13 1.334(4) . ?
C12 C14 1.553(4) . ?
C13 C15 1.506(4) . ?
C13 C20 1.519(4) . ?
C14 C15 1.523(3) . ?
C14 C16 1.530(4) . ?
C15 C18 1.552(4) . ?
C16 H18 0.9900 . ?
C16 H19 0.9900 . ?
C17 C22 1.505(4) . ?
C17 C26 1.524(4) . ?
C17 C18 1.544(4) . ?
C18 C19 1.521(3) . ?
C18 H23 1.0000 . ?
C19 C20 1.517(4) . ?
C20 C21 1.528(4) . ?
C20 H24 1.0000 . ?
C21 C22 1.338(4) . ?
C21 H25 0.9500 . ?
C22 H26 0.9500 . ?
C23 H9 0.9800 . ?
C23 H10 0.9800 . ?
C23 H11 0.9800 . ?
C24 H12 0.9800 . ?
C24 H13 0.9800 . ?
C24 H14 0.9800 . ?
C25 H15 0.9800 . ?
C25 H16 0.9800 . ?
C25 H17 0.9800 . ?
C26 H20 0.9800 . ?
C26 H21 0.9800 . ?
C26 H22 0.9800 . ?
C27 C28 1.498(5) . ?
C27 H33 0.9900 . ?
C27 H34 0.9900 . ?
C28 H35 0.9900 . ?
C28 H36 0.9900 . ?
C29 H27 0.9800 . ?
C29 H28 0.9800 . ?
C29 H29 0.9800 . ?
C30 H30 0.9800 . ?
C30 H31 0.9800 . ?
C30 H32 0.9800 . ?
C31 H40 0.9800 . ?
C31 H41 0.9800 . ?
C31 H42 0.9800 . ?
C32 H37 0.9800 . ?
C32 H38 0.9800 . ?
C32 H39 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 O1 C3 C5 1.0(5) . . . . ?
C1 O1 C3 C4 -179.9(3) . . . . ?
C2 O2 C4 C6 16.9(4) . . . . ?
C2 O2 C4 C3 -164.0(3) . . . . ?
O1 C3 C4 O2 -2.7(4) . . . . ?
C5 C3 C4 O2 176.4(3) . . . . ?
O1 C3 C4 C6 176.4(3) . . . . ?
C5 C3 C4 C6 -4.5(5) . . . . ?
O1 C3 C5 C7 -178.7(3) . . . . ?
C4 C3 C5 C7 2.4(4) . . . . ?
O2 C4 C6 C8 -179.0(3) . . . . ?
C3 C4 C6 C8 2.0(4) . . . . ?
C3 C5 C7 C8 2.1(4) . . . . ?
C3 C5 C7 C9 -172.8(3) . . . . ?
C5 C7 C8 C6 -4.7(4) . . . . ?
C9 C7 C8 C6 171.1(2) . . . . ?
C5 C7 C8 C11 179.7(3) . . . . ?
C9 C7 C8 C11 -4.5(3) . . . . ?
C4 C6 C8 C7 2.5(4) . . . . ?
C4 C6 C8 C11 177.3(3) . . . . ?
C5 C7 C9 O3 0.5(5) . . . . ?
C8 C7 C9 O3 -174.9(3) . . . . ?
C5 C7 C9 C10 -179.3(3) . . . . ?
C8 C7 C9 C10 5.3(3) . . . . ?
O3 C9 C10 C12 -13.0(5) . . . . ?
C7 C9 C10 C12 166.7(3) . . . . ?
O3 C9 C10 C11 176.2(3) . . . . ?
C7 C9 C10 C11 -4.0(3) . . . . ?
C7 C8 C11 C13 -175.1(3) . . . . ?
C6 C8 C11 C13 9.8(5) . . . . ?
C7 C8 C11 C10 1.9(3) . . . . ?
C6 C8 C11 C10 -173.2(3) . . . . ?
C12 C10 C11 C13 7.5(4) . . . . ?
C9 C10 C11 C13 178.9(2) . . . . ?
C12 C10 C11 C8 -170.0(3) . . . . ?
C9 C10 C11 C8 1.4(3) . . . . ?
C11 C10 C12 C14 3.5(4) . . . . ?
C9 C10 C12 C14 -165.7(3) . . . . ?
C11 C10 C12 Si1 177.9(2) . . . . ?
C9 C10 C12 Si1 8.6(4) . . . . ?
C8 C11 C13 C15 -175.6(3) . . . . ?
C10 C11 C13 C15 7.7(4) . . . . ?
C8 C11 C13 C20 16.0(5) . . . . ?
C10 C11 C13 C20 -160.7(3) . . . . ?
Os1 O7 C14 C15 -34.3(2) . . . . ?
Os1 O7 C14 C16 -152.39(16) . . . . ?
Os1 O7 C14 C12 90.6(2) . . . . ?
C10 C12 C14 O7 -148.5(2) . . . . ?
Si1 C12 C14 O7 37.0(3) . . . . ?
C10 C12 C14 C15 -27.4(3) . . . . ?
Si1 C12 C14 C15 158.10(19) . . . . ?
C10 C12 C14 C16 92.2(3) . . . . ?
Si1 C12 C14 C16 -82.2(2) . . . . ?
Os1 O6 C15 C13 -161.07(16) . . . . ?
Os1 O6 C15 C14 -36.7(2) . . . . ?
Os1 O6 C15 C18 87.70(19) . . . . ?
C11 C13 C15 O6 88.4(3) . . . . ?
C20 C13 C15 O6 -100.9(2) . . . . ?
C11 C13 C15 C14 -32.2(4) . . . . ?
C20 C13 C15 C14 138.5(2) . . . . ?
C11 C13 C15 C18 -157.9(2) . . . . ?
C20 C13 C15 C18 12.8(3) . . . . ?
O7 C14 C15 O6 45.5(3) . . . . ?
C16 C14 C15 O6 163.5(2) . . . . ?
C12 C14 C15 O6 -79.2(3) . . . . ?
O7 C14 C15 C13 165.7(2) . . . . ?
C16 C14 C15 C13 -76.3(3) . . . . ?
C12 C14 C15 C13 41.1(3) . . . . ?
O7 C14 C15 C18 -74.5(3) . . . . ?
C16 C14 C15 C18 43.5(3) . . . . ?
C12 C14 C15 C18 160.9(2) . . . . ?
C17 O4 C16 C14 63.0(3) . . . . ?
O7 C14 C16 O4 65.3(3) . . . . ?
C15 C14 C16 O4 -50.9(3) . . . . ?
C12 C14 C16 O4 -173.0(2) . . . . ?
C16 O4 C17 C22 63.1(3) . . . . ?
C16 O4 C17 C26 -179.4(2) . . . . ?
C16 O4 C17 C18 -61.1(3) . . . . ?
O4 C17 C18 C19 161.1(2) . . . . ?
C22 C17 C18 C19 36.8(3) . . . . ?
C26 C17 C18 C19 -84.8(3) . . . . ?
O4 C17 C18 C15 51.4(3) . . . . ?
C22 C17 C18 C15 -73.0(3) . . . . ?
C26 C17 C18 C15 165.5(2) . . . . ?
O6 C15 C18 C19 78.7(2) . . . . ?
C13 C15 C18 C19 -35.2(2) . . . . ?
C14 C15 C18 C19 -160.8(2) . . . . ?
O6 C15 C18 C17 -166.4(2) . . . . ?
C13 C15 C18 C17 79.7(3) . . . . ?
C14 C15 C18 C17 -46.0(3) . . . . ?
C17 C18 C19 O5 105.9(3) . . . . ?
C15 C18 C19 O5 -136.2(3) . . . . ?
C17 C18 C19 C20 -72.0(3) . . . . ?
C15 C18 C19 C20 45.8(3) . . . . ?
O5 C19 C20 C13 144.1(3) . . . . ?
C18 C19 C20 C13 -37.9(3) . . . . ?
O5 C19 C20 C21 -106.7(3) . . . . ?
C18 C19 C20 C21 71.2(2) . . . . ?
C11 C13 C20 C19 -175.8(3) . . . . ?
C15 C13 C20 C19 14.9(3) . . . . ?
C11 C13 C20 C21 76.2(3) . . . . ?
C15 C13 C20 C21 -93.1(3) . . . . ?
C19 C20 C21 C22 -40.7(3) . . . . ?
C13 C20 C21 C22 65.9(3) . . . . ?
C20 C21 C22 C17 7.8(4) . . . . ?
O4 C17 C22 C21 -127.1(3) . . . . ?
C26 C17 C22 C21 117.8(3) . . . . ?
C18 C17 C22 C21 -5.1(4) . . . . ?
C29 N1 C27 C28 166.2(3) . . . . ?
C30 N1 C27 C28 -77.2(3) . . . . ?
Os1 N1 C27 C28 45.4(3) . . . . ?
C31 N2 C28 C27 -84.3(3) . . . . ?
C32 N2 C28 C27 157.8(3) . . . . ?
Os1 N2 C28 C27 37.8(3) . . . . ?
N1 C27 C28 N2 -59.1(4) . . . . ?
