# Electronic Supplementary Material (ESI) for New Journal of Chemistry
# This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012
data_global
_journal_name_full 'New J.Chem.'
_journal_coden_Cambridge 0440
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Bunz, Uwe H. F.'
_publ_contact_author_address
;
Organisch-Chemisches Institut
Ruprecht-Karls-Universit\"at Heidelberg
Im Neuenheimer Feld 270
D-69120 Heidelberg
Germany
;
_publ_contact_author_phone '049 6221 54- 8401'
_publ_contact_author_fax '049 6221 54- 8404'
_publ_contact_author_email uwe.bunz@oci.uni-heidelberg.de
_publ_requested_coeditor_name ?
#====================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
Photophysical property trends for a homologous series
of bis-ethynyl-substituted benzochalcogendiazoles
;
loop_
_publ_author_name
_publ_author_address
B.A.Coombs
; Organisch-Chemisches Institut
Ruprecht-Karls-Universit\"at Heidelberg
Im Neuenheimer Feld 270
69120 Heidelberg
Germany
;
B.D.Lindner
; Organisch-Chemisches Institut
Ruprecht-Karls-Universit\"at Heidelberg
Im Neuenheimer Feld 270
69120 Heidelberg
Germany
;
F.Rominger
; Organisch-Chemisches Institut
Ruprecht-Karls-Universit\"at Heidelberg
Im Neuenheimer Feld 270
69120 Heidelberg
Germany
;
A.Beeby
; Department of Chemistry
Durham University Science Site
South Road
Durham, DH1 3LE
UK
;
U.H.F.Bunz
; Organisch-Chemisches Institut
Ruprecht-Karls-Universit\"at Heidelberg
Im Neuenheimer Feld 270
69120 Heidelberg
Germany
;
# Attachment '- BLI BC 2011.cif'
#TrackingRef '- BLI BC 2011.cif'
#==================================================================
data_bc1
_database_code_depnum_ccdc_archive 'CCDC 846082'
#TrackingRef '- BLI BC 2011.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C28 H44 N2 O Si2'
_chemical_formula_weight 480.83
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/c
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
_cell_length_a 14.8274(3)
_cell_length_b 15.2591(3)
_cell_length_c 14.0991(3)
_cell_angle_alpha 90.00
_cell_angle_beta 106.703(1)
_cell_angle_gamma 90.00
_cell_volume 3055.37(11)
_cell_formula_units_Z 4
_cell_measurement_temperature 200(2)
_cell_measurement_reflns_used 4466
_cell_measurement_theta_min ?
_cell_measurement_theta_max ?
_exptl_crystal_description polyhedron
_exptl_crystal_colour colourless
_exptl_crystal_size_max 0.42
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.28
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.045
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1048
_exptl_absorpt_coefficient_mu 0.136
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9450
_exptl_absorpt_correction_T_max 0.9628
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 200(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART CCD'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 18484
_diffrn_reflns_av_R_equivalents 0.0599
_diffrn_reflns_av_sigmaI/netI 0.0418
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.43
_diffrn_reflns_theta_max 21.51
_reflns_number_total 3523
_reflns_number_gt 2512
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker SMART'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1098P)^2^+1.4638P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3523
_refine_ls_number_parameters 389
_refine_ls_number_restraints 576
_refine_ls_R_factor_all 0.0906
_refine_ls_R_factor_gt 0.0628
_refine_ls_wR_factor_ref 0.1935
_refine_ls_wR_factor_gt 0.1687
_refine_ls_goodness_of_fit_ref 1.041
_refine_ls_restrained_S_all 1.183
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
C1 C 0.6297(3) -0.1318(3) 0.1976(3) 0.0576(11) Uani 1 1 d . . .
C2 C 0.5907(3) -0.0653(3) 0.2068(3) 0.0640(12) Uani 1 1 d . . .
C3 C 0.8476(3) -0.4434(3) 0.1920(3) 0.0618(12) Uani 1 1 d . A .
C4 C 0.8943(3) -0.5082(3) 0.1996(4) 0.0793(14) Uani 1 1 d . . .
C11 C 0.6811(3) -0.2100(2) 0.1939(3) 0.0479(10) Uani 1 1 d . A .
C12 C 0.7298(3) -0.2547(2) 0.2822(3) 0.0471(10) Uani 1 1 d . . .
N13 N 0.7333(3) -0.2349(3) 0.3736(3) 0.0728(11) Uani 1 1 d . . .
O1 O 0.7901(3) -0.2994(2) 0.4291(2) 0.0967(12) Uani 1 1 d . . .
N14 N 0.8218(3) -0.3580(3) 0.3718(3) 0.0777(11) Uani 1 1 d . . .
C15 C 0.7845(3) -0.3304(2) 0.2808(3) 0.0498(10) Uani 1 1 d . A .
C16 C 0.7930(3) -0.3666(2) 0.1910(3) 0.0509(10) Uani 1 1 d . . .
C17 C 0.7454(3) -0.3232(3) 0.1080(3) 0.0633(12) Uani 1 1 d . A .
H17 H 0.7486 -0.3447 0.0458 0.076 Uiso 1 1 calc R . .
C18 C 0.6908(3) -0.2469(3) 0.1095(3) 0.0622(12) Uani 1 1 d . . .
H18 H 0.6593 -0.2201 0.0481 0.075 Uiso 1 1 calc R A .
Si1 Si 0.53974(9) 0.04010(8) 0.22971(9) 0.0700(5) Uani 1 1 d D . .
C31 C 0.4110(3) 0.0235(3) 0.2076(4) 0.0930(17) Uani 1 1 d D . .
H31 H 0.3840 0.0812 0.2194 0.112 Uiso 1 1 calc R . .
C32 C 0.3875(4) -0.0421(4) 0.2782(5) 0.138(3) Uani 1 1 d D . .
H32A H 0.4198 -0.0254 0.3467 0.206 Uiso 1 1 calc R . .
H32B H 0.4082 -0.1007 0.2651 0.206 Uiso 1 1 calc R . .
H32C H 0.3193 -0.0426 0.2684 0.206 Uiso 1 1 calc R . .
C33 C 0.3618(4) -0.0025(5) 0.1009(4) 0.133(2) Uani 1 1 d D . .
H33A H 0.3761 0.0407 0.0558 0.200 Uiso 1 1 calc R . .
H33B H 0.2937 -0.0046 0.0908 0.200 Uiso 1 1 calc R . .
H33C H 0.3841 -0.0604 0.0875 0.200 Uiso 1 1 calc R . .
C34 C 0.6023(4) 0.0716(3) 0.3583(3) 0.1006(18) Uani 1 1 d D . .
H34 H 0.6617 0.1005 0.3545 0.121 Uiso 1 1 calc R . .
C35 C 0.6332(5) -0.0025(4) 0.4296(4) 0.141(3) Uani 1 1 d D . .
H35A H 0.6652 -0.0469 0.4007 0.211 Uiso 1 1 calc R . .
H35B H 0.5781 -0.0288 0.4436 0.211 Uiso 1 1 calc R . .
H35C H 0.6765 0.0195 0.4913 0.211 Uiso 1 1 calc R . .
C36 C 0.5503(5) 0.1414(4) 0.4009(4) 0.146(3) Uani 1 1 d D . .
H36A H 0.5290 0.1886 0.3524 0.219 Uiso 1 1 calc R . .
H36B H 0.5929 0.1655 0.4618 0.219 Uiso 1 1 calc R . .
H36C H 0.4957 0.1148 0.4156 0.219 Uiso 1 1 calc R . .
C37 C 0.5608(3) 0.1197(3) 0.1375(4) 0.0911(16) Uani 1 1 d D . .
H37 H 0.5269 0.0952 0.0711 0.109 Uiso 1 1 calc R . .
C38 C 0.6620(4) 0.1264(5) 0.1386(6) 0.153(3) Uani 1 1 d D . .
H38A H 0.6876 0.0675 0.1361 0.229 Uiso 1 1 calc R . .
H38B H 0.6981 0.1560 0.1993 0.229 Uiso 1 1 calc R . .
H38C H 0.6665 0.1601 0.0809 0.229 Uiso 1 1 calc R . .
C39 C 0.5168(5) 0.2094(3) 0.1420(5) 0.129(2) Uani 1 1 d D . .
H39A H 0.4511 0.2020 0.1418 0.194 Uiso 1 1 calc R . .
H39B H 0.5192 0.2442 0.0843 0.194 Uiso 1 1 calc R . .
H39C H 0.5518 0.2397 0.2027 0.194 Uiso 1 1 calc R . .
Si2 Si 0.9546(5) -0.6170(5) 0.2200(5) 0.128(3) Uani 0.593(7) 1 d PDU A 1
C41 C 1.0845(5) -0.5964(5) 0.2538(6) 0.094(3) Uani 0.593(7) 1 d PDU A 1
H41 H 1.1146 -0.6556 0.2601 0.113 Uiso 0.593(7) 1 calc PR A 1
C42 C 1.1134(8) -0.5503(11) 0.1726(9) 0.184(8) Uani 0.593(7) 1 d PDU A 1
H42A H 1.0854 -0.5803 0.1095 0.277 Uiso 0.593(7) 1 calc PR A 1
H42B H 1.1822 -0.5512 0.1877 0.277 Uiso 0.593(7) 1 calc PR A 1
H42C H 1.0914 -0.4895 0.1677 0.277 Uiso 0.593(7) 1 calc PR A 1
C43 C 1.1238(8) -0.5531(11) 0.3527(8) 0.136(5) Uani 0.593(7) 1 d PDU A 1
H43A H 1.1042 -0.5859 0.4032 0.204 Uiso 0.593(7) 1 calc PR A 1
H43B H 1.1002 -0.4929 0.3496 0.204 Uiso 0.593(7) 1 calc PR A 1
H43C H 1.1927 -0.5523 0.3698 0.204 Uiso 0.593(7) 1 calc PR A 1
C44 C 0.9172(8) -0.6722(9) 0.0951(9) 0.329(13) Uani 0.593(7) 1 d PDU A 1
H44 H 0.9455 -0.6378 0.0505 0.394 Uiso 0.593(7) 1 calc PR A 1
C45 C 0.958(2) -0.7644(15) 0.1009(19) 0.56(4) Uani 0.593(7) 1 d PDU A 1
H45A H 1.0244 -0.7633 0.1395 0.846 Uiso 0.593(7) 1 calc PR A 1
H45B H 0.9523 -0.7858 0.0340 0.846 Uiso 0.593(7) 1 calc PR A 1
H45C H 0.9231 -0.8034 0.1331 0.846 Uiso 0.593(7) 1 calc PR A 1
C46 C 0.8125(10) -0.6711(18) 0.0489(16) 0.36(3) Uani 0.593(7) 1 d PDU A 1
H46A H 0.7906 -0.6103 0.0381 0.534 Uiso 0.593(7) 1 calc PR A 1
H46B H 0.7816 -0.7003 0.0931 0.534 Uiso 0.593(7) 1 calc PR A 1
H46C H 0.7970 -0.7021 -0.0147 0.534 Uiso 0.593(7) 1 calc PR A 1
C47 C 0.9205(8) -0.6822(7) 0.3129(11) 0.314(13) Uani 0.593(7) 1 d PDU A 1
H47 H 0.8655 -0.7150 0.2698 0.377 Uiso 0.593(7) 1 calc PR A 1
C48 C 0.8761(18) -0.6381(16) 0.3800(15) 0.48(3) Uani 0.593(7) 1 d PDU A 1
H48A H 0.8318 -0.5937 0.3434 0.723 Uiso 0.593(7) 1 calc PR A 1
H48B H 0.9245 -0.6098 0.4336 0.723 Uiso 0.593(7) 1 calc PR A 1
H48C H 0.8420 -0.6813 0.4082 0.723 Uiso 0.593(7) 1 calc PR A 1
C49 C 0.9852(15) -0.7569(11) 0.3568(17) 0.349(18) Uani 0.593(7) 1 d PDU A 1
H49A H 0.9984 -0.7912 0.3036 0.523 Uiso 0.593(7) 1 calc PR A 1
H49B H 0.9551 -0.7945 0.3952 0.523 Uiso 0.593(7) 1 calc PR A 1
H49C H 1.0443 -0.7337 0.4003 0.523 Uiso 0.593(7) 1 calc PR A 1
Si2B Si 0.9742(6) -0.6008(6) 0.2191(5) 0.091(2) Uani 0.407(7) 1 d PDU A 2
C41B C 0.8917(7) -0.6938(6) 0.1808(10) 0.133(6) Uani 0.407(7) 1 d PDU A 2
H41B H 0.8482 -0.6913 0.2234 0.160 Uiso 0.407(7) 1 calc PR A 2
C42B C 0.8303(15) -0.6874(13) 0.0749(15) 0.27(2) Uani 0.407(7) 1 d PDU A 2
H42D H 0.8020 -0.6290 0.0631 0.398 Uiso 0.407(7) 1 calc PR A 2
H42E H 0.7804 -0.7317 0.0631 0.398 Uiso 0.407(7) 1 calc PR A 2
H42F H 0.8687 -0.6975 0.0298 0.398 Uiso 0.407(7) 1 calc PR A 2
C43B C 0.9407(11) -0.7830(6) 0.2003(18) 0.170(10) Uani 0.407(7) 1 d PDU A 2
H43D H 0.9814 -0.7852 0.2687 0.255 Uiso 0.407(7) 1 calc PR A 2
H43E H 0.9788 -0.7914 0.1546 0.255 Uiso 0.407(7) 1 calc PR A 2
H43F H 0.8933 -0.8295 0.1901 0.255 Uiso 0.407(7) 1 calc PR A 2
C44B C 1.0591(10) -0.5927(9) 0.1462(10) 0.136(6) Uani 0.407(7) 1 d PDU A 2
H44B H 1.1142 -0.6291 0.1826 0.163 Uiso 0.407(7) 1 calc PR A 2
C45B C 1.0254(18) -0.6321(17) 0.0438(12) 0.258(15) Uani 0.407(7) 1 d PDU A 2
H45D H 1.0005 -0.6910 0.0480 0.387 Uiso 0.407(7) 1 calc PR A 2
H45E H 1.0782 -0.6357 0.0151 0.387 Uiso 0.407(7) 1 calc PR A 2
H45F H 0.9758 -0.5951 0.0018 0.387 Uiso 0.407(7) 1 calc PR A 2
C46B C 1.0979(15) -0.5012(10) 0.1430(19) 0.214(13) Uani 0.407(7) 1 d PDU A 2
H46D H 1.1192 -0.4773 0.2103 0.321 Uiso 0.407(7) 1 calc PR A 2
H46E H 1.0486 -0.4635 0.1017 0.321 Uiso 0.407(7) 1 calc PR A 2
H46F H 1.1511 -0.5038 0.1149 0.321 Uiso 0.407(7) 1 calc PR A 2
C47B C 1.0307(10) -0.5989(10) 0.3545(6) 0.170(7) Uani 0.407(7) 1 d PDU A 2
H47B H 1.0685 -0.6540 0.3700 0.204 Uiso 0.407(7) 1 calc PR A 2
C48B C 1.100(2) -0.5251(18) 0.3890(13) 0.33(2) Uani 0.407(7) 1 d PDU A 2
H48D H 1.1446 -0.5245 0.3495 0.498 Uiso 0.407(7) 1 calc PR A 2
H48E H 1.1343 -0.5337 0.4589 0.498 Uiso 0.407(7) 1 calc PR A 2
H48F H 1.0661 -0.4693 0.3809 0.498 Uiso 0.407(7) 1 calc PR A 2
C49B C 0.9600(15) -0.6038(18) 0.4134(10) 0.33(2) Uani 0.407(7) 1 d PDU A 2
H49D H 0.9148 -0.6508 0.3869 0.496 Uiso 0.407(7) 1 calc PR A 2
H49E H 0.9265 -0.5478 0.4084 0.496 Uiso 0.407(7) 1 calc PR A 2
H49F H 0.9930 -0.6159 0.4830 0.496 Uiso 0.407(7) 1 calc PR A 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
C1 0.060(3) 0.059(3) 0.056(3) 0.004(2) 0.021(2) 0.006(2)
C2 0.061(3) 0.066(3) 0.068(3) 0.004(2) 0.022(2) 0.012(2)
C3 0.057(3) 0.052(3) 0.076(3) 0.000(2) 0.019(2) 0.002(2)
C4 0.063(3) 0.058(3) 0.112(4) -0.004(3) 0.018(3) 0.009(3)
C11 0.050(2) 0.044(2) 0.052(3) 0.0011(19) 0.019(2) 0.0026(19)
C12 0.050(2) 0.050(2) 0.045(2) 0.0001(19) 0.0196(19) -0.002(2)
N13 0.088(3) 0.077(3) 0.054(2) 0.003(2) 0.022(2) 0.015(2)
O1 0.132(3) 0.108(3) 0.0480(18) 0.0094(19) 0.022(2) 0.037(2)
N14 0.095(3) 0.079(3) 0.057(2) 0.013(2) 0.018(2) 0.021(2)
C15 0.053(2) 0.045(2) 0.054(3) 0.008(2) 0.018(2) 0.0011(19)
C16 0.055(2) 0.042(2) 0.059(3) 0.004(2) 0.021(2) 0.004(2)
C17 0.084(3) 0.053(3) 0.057(3) -0.004(2) 0.026(2) 0.012(2)
C18 0.079(3) 0.059(3) 0.048(3) 0.008(2) 0.018(2) 0.015(2)
Si1 0.0737(9) 0.0611(9) 0.0785(9) 0.0051(6) 0.0270(7) 0.0237(6)
C31 0.078(4) 0.072(3) 0.135(5) 0.011(3) 0.041(4) 0.027(3)
C32 0.116(5) 0.120(5) 0.205(8) 0.023(5) 0.093(5) 0.008(4)
C33 0.088(4) 0.130(6) 0.164(7) 0.001(5) 0.009(4) 0.005(4)
C34 0.115(4) 0.097(4) 0.090(4) -0.012(3) 0.029(3) 0.042(3)
C35 0.193(7) 0.145(6) 0.076(4) 0.008(4) 0.027(4) 0.067(6)
C36 0.194(7) 0.129(6) 0.111(5) -0.031(4) 0.040(5) 0.072(5)
C37 0.091(4) 0.071(3) 0.114(4) 0.016(3) 0.033(3) 0.012(3)
C38 0.135(6) 0.160(7) 0.181(7) 0.059(6) 0.074(6) 0.008(5)
C39 0.169(7) 0.080(4) 0.146(6) 0.036(4) 0.056(5) 0.030(4)
Si2 0.058(3) 0.061(3) 0.245(6) -0.009(3) 0.014(3) 0.023(2)
C41 0.078(6) 0.086(7) 0.114(7) 0.010(5) 0.021(5) 0.033(5)
C42 0.129(12) 0.22(2) 0.232(13) 0.111(15) 0.099(11) 0.088(13)
C43 0.117(9) 0.105(10) 0.169(10) -0.021(8) 0.013(8) -0.022(7)
C44 0.185(14) 0.25(2) 0.432(19) -0.264(18) -0.104(17) 0.126(15)
C45 0.54(5) 0.34(3) 0.58(6) -0.31(4) -0.21(4) 0.29(4)
C46 0.199(18) 0.26(3) 0.46(4) -0.09(3) -0.14(3) 0.02(2)
C47 0.24(2) 0.120(12) 0.67(3) 0.217(17) 0.26(3) 0.105(13)
C48 0.41(4) 0.62(5) 0.53(4) 0.45(4) 0.32(3) 0.43(4)
C49 0.27(2) 0.200(19) 0.60(5) 0.23(3) 0.17(3) 0.133(18)
Si2B 0.062(4) 0.073(4) 0.135(5) 0.006(3) 0.022(3) 0.020(3)
C41B 0.095(10) 0.028(7) 0.290(19) 0.009(10) 0.077(11) 0.019(6)
C42B 0.14(2) 0.111(19) 0.43(4) -0.10(2) -0.10(3) 0.052(18)
C43B 0.124(14) 0.031(7) 0.36(3) 0.008(12) 0.083(16) 0.022(7)
C44B 0.089(13) 0.117(12) 0.227(16) -0.021(13) 0.085(13) 0.006(9)
C45B 0.31(4) 0.34(3) 0.158(18) 0.004(18) 0.12(2) -0.02(3)
C46B 0.16(2) 0.140(16) 0.39(4) 0.095(17) 0.15(2) 0.020(14)
C47B 0.18(2) 0.156(16) 0.142(10) 0.037(12) 0.006(9) 0.079(13)
C48B 0.52(5) 0.14(3) 0.18(3) 0.02(2) -0.15(2) -0.03(3)
C49B 0.36(3) 0.47(4) 0.205(18) 0.24(3) 0.16(2) 0.36(3)
_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
C1 C2 1.192(6) . ?
C1 C11 1.425(6) . ?
C2 Si1 1.845(5) . ?
C3 C4 1.194(6) . ?
C3 C16 1.423(6) . ?
C4 Si2B 1.813(11) . ?
C4 Si2 1.867(9) . ?
C11 C18 1.361(5) . ?
C11 C12 1.421(5) . ?
C12 N13 1.311(5) . ?
C12 C15 1.415(5) . ?
N13 O1 1.383(5) . ?
O1 N14 1.376(5) . ?
N14 C15 1.312(5) . ?
C15 C16 1.420(5) . ?
C16 C17 1.353(5) . ?
C17 C18 1.422(6) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
Si1 C34 1.847(4) . ?
Si1 C31 1.860(4) . ?
Si1 C37 1.870(4) . ?
C31 C32 1.522(5) . ?
C31 C33 1.524(6) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.495(6) . ?
C34 C36 1.536(5) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C38 1.499(6) . ?
C37 C39 1.526(5) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
Si2 C47 1.827(7) . ?
Si2 C41 1.873(7) . ?
Si2 C44 1.887(7) . ?
C41 C43 1.500(7) . ?
C41 C42 1.507(7) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C46 1.501(9) . ?
C44 C45 1.523(9) . ?
C44 H44 1.0000 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.464(8) . ?
C47 C49 1.505(8) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
Si2B C44B 1.843(8) . ?
Si2B C41B 1.851(7) . ?
Si2B C47B 1.852(8) . ?
C41B C42B 1.512(9) . ?
C41B C43B 1.530(8) . ?
C41B H41B 1.0000 . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?
C44B C45B 1.511(8) . ?
C44B C46B 1.515(9) . ?
C44B H44B 1.0000 . ?
C45B H45D 0.9800 . ?
C45B H45E 0.9800 . ?
C45B H45F 0.9800 . ?
C46B H46D 0.9800 . ?
C46B H46E 0.9800 . ?
C46B H46F 0.9800 . ?
C47B C48B 1.506(8) . ?
C47B C49B 1.515(8) . ?
C47B H47B 1.0000 . ?
C48B H48D 0.9800 . ?
C48B H48E 0.9800 . ?
C48B H48F 0.9800 . ?
C49B H49D 0.9800 . ?
C49B H49E 0.9800 . ?
C49B H49F 0.9800 . ?
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
C2 C1 C11 175.7(4) . . ?
C1 C2 Si1 175.0(4) . . ?
C4 C3 C16 175.6(5) . . ?
C3 C4 Si2B 174.5(5) . . ?
C3 C4 Si2 171.5(5) . . ?
Si2B C4 Si2 11.9(4) . . ?
C18 C11 C12 114.3(3) . . ?
C18 C11 C1 124.9(4) . . ?
C12 C11 C1 120.8(3) . . ?
N13 C12 C15 110.0(3) . . ?
N13 C12 C11 128.1(4) . . ?
C15 C12 C11 121.9(3) . . ?
C12 N13 O1 103.8(3) . . ?
N14 O1 N13 112.6(3) . . ?
C15 N14 O1 104.3(3) . . ?
N14 C15 C12 109.3(4) . . ?
N14 C15 C16 128.8(4) . . ?
C12 C15 C16 121.9(4) . . ?
C17 C16 C15 115.0(4) . . ?
C17 C16 C3 124.5(4) . . ?
C15 C16 C3 120.5(4) . . ?
C16 C17 C18 123.0(4) . . ?
C16 C17 H17 118.5 . . ?
C18 C17 H17 118.5 . . ?
C11 C18 C17 123.8(4) . . ?
C11 C18 H18 118.1 . . ?
C17 C18 H18 118.1 . . ?
C2 Si1 C34 106.45(19) . . ?
C2 Si1 C31 107.7(2) . . ?
C34 Si1 C31 113.7(2) . . ?
C2 Si1 C37 106.6(2) . . ?
C34 Si1 C37 112.1(2) . . ?
C31 Si1 C37 109.9(2) . . ?
C32 C31 C33 109.8(4) . . ?
C32 C31 Si1 113.4(3) . . ?
C33 C31 Si1 112.2(3) . . ?
C32 C31 H31 107.0 . . ?
C33 C31 H31 107.0 . . ?
Si1 C31 H31 107.0 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C36 110.7(4) . . ?
C35 C34 Si1 115.7(4) . . ?
C36 C34 Si1 113.4(3) . . ?
C35 C34 H34 105.3 . . ?
C36 C34 H34 105.3 . . ?
Si1 C34 H34 105.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C38 C37 C39 112.2(5) . . ?
C38 C37 Si1 113.8(4) . . ?
C39 C37 Si1 113.3(3) . . ?
C38 C37 H37 105.5 . . ?
C39 C37 H37 105.5 . . ?
Si1 C37 H37 105.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C47 Si2 C4 112.1(5) . . ?
C47 Si2 C41 112.6(4) . . ?
C4 Si2 C41 107.6(4) . . ?
C47 Si2 C44 111.0(5) . . ?
C4 Si2 C44 104.7(5) . . ?
C41 Si2 C44 108.5(4) . . ?
C43 C41 C42 112.4(7) . . ?
C43 C41 Si2 114.0(6) . . ?
C42 C41 Si2 112.4(5) . . ?
C43 C41 H41 105.7 . . ?
C42 C41 H41 105.7 . . ?
Si2 C41 H41 105.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C46 C44 C45 112.2(9) . . ?
C46 C44 Si2 112.9(7) . . ?
C45 C44 Si2 110.9(7) . . ?
C46 C44 H44 106.8 . . ?
C45 C44 H44 106.8 . . ?
Si2 C44 H44 106.8 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C49 115.7(8) . . ?
C48 C47 Si2 118.8(7) . . ?
C49 C47 Si2 115.6(6) . . ?
C48 C47 H47 100.5 . . ?
C49 C47 H47 100.5 . . ?
Si2 C47 H47 100.5 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C4 Si2B C44B 112.6(6) . . ?
C4 Si2B C41B 101.8(5) . . ?
C44B Si2B C41B 112.9(5) . . ?
C4 Si2B C47B 103.1(6) . . ?
C44B Si2B C47B 113.2(6) . . ?
C41B Si2B C47B 112.2(5) . . ?
C42B C41B C43B 110.8(8) . . ?
C42B C41B Si2B 113.5(7) . . ?
C43B C41B Si2B 112.9(6) . . ?
C42B C41B H41B 106.4 . . ?
C43B C41B H41B 106.4 . . ?
Si2B C41B H41B 106.4 . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41B C43B H43D 109.5 . . ?
C41B C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C41B C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C45B C44B C46B 111.2(8) . . ?
C45B C44B Si2B 114.6(7) . . ?
C46B C44B Si2B 113.9(7) . . ?
C45B C44B H44B 105.4 . . ?
C46B C44B H44B 105.4 . . ?
Si2B C44B H44B 105.4 . . ?
C44B C45B H45D 109.5 . . ?
C44B C45B H45E 109.5 . . ?
H45D C45B H45E 109.5 . . ?
C44B C45B H45F 109.5 . . ?
H45D C45B H45F 109.5 . . ?
H45E C45B H45F 109.5 . . ?
C44B C46B H46D 109.5 . . ?
C44B C46B H46E 109.5 . . ?
H46D C46B H46E 109.5 . . ?
C44B C46B H46F 109.5 . . ?
H46D C46B H46F 109.5 . . ?
H46E C46B H46F 109.5 . . ?
C48B C47B C49B 112.0(9) . . ?
C48B C47B Si2B 114.1(7) . . ?
C49B C47B Si2B 112.6(7) . . ?
C48B C47B H47B 105.7 . . ?
C49B C47B H47B 105.7 . . ?
Si2B C47B H47B 105.7 . . ?
C47B C48B H48D 109.5 . . ?
C47B C48B H48E 109.5 . . ?
H48D C48B H48E 109.5 . . ?
C47B C48B H48F 109.5 . . ?
H48D C48B H48F 109.5 . . ?
H48E C48B H48F 109.5 . . ?
C47B C49B H49D 109.5 . . ?
C47B C49B H49E 109.5 . . ?
H49D C49B H49E 109.5 . . ?
C47B C49B H49F 109.5 . . ?
H49D C49B H49F 109.5 . . ?
H49E C49B H49F 109.5 . . ?
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
C11 C1 C2 Si1 15(10) . . . . ?
C16 C3 C4 Si2B -60(9) . . . . ?
C16 C3 C4 Si2 55(8) . . . . ?
C2 C1 C11 C18 -149(6) . . . . ?
C2 C1 C11 C12 29(6) . . . . ?
C18 C11 C12 N13 -179.8(4) . . . . ?
C1 C11 C12 N13 2.0(6) . . . . ?
C18 C11 C12 C15 0.8(5) . . . . ?
C1 C11 C12 C15 -177.4(4) . . . . ?
C15 C12 N13 O1 -0.4(4) . . . . ?
C11 C12 N13 O1 -179.9(4) . . . . ?
C12 N13 O1 N14 0.4(5) . . . . ?
N13 O1 N14 C15 -0.3(5) . . . . ?
O1 N14 C15 C12 0.1(4) . . . . ?
O1 N14 C15 C16 -179.6(4) . . . . ?
N13 C12 C15 N14 0.2(5) . . . . ?
C11 C12 C15 N14 179.7(4) . . . . ?
N13 C12 C15 C16 179.9(4) . . . . ?
C11 C12 C15 C16 -0.6(6) . . . . ?
N14 C15 C16 C17 179.8(4) . . . . ?
C12 C15 C16 C17 0.1(6) . . . . ?
N14 C15 C16 C3 0.3(6) . . . . ?
C12 C15 C16 C3 -179.3(4) . . . . ?
C4 C3 C16 C17 -174(6) . . . . ?
C4 C3 C16 C15 5(6) . . . . ?
C15 C16 C17 C18 0.1(6) . . . . ?
C3 C16 C17 C18 179.5(4) . . . . ?
C12 C11 C18 C17 -0.5(6) . . . . ?
C1 C11 C18 C17 177.6(4) . . . . ?
C16 C17 C18 C11 0.1(7) . . . . ?
C1 C2 Si1 C34 -23(5) . . . . ?
C1 C2 Si1 C31 -145(5) . . . . ?
C1 C2 Si1 C37 97(5) . . . . ?
C2 Si1 C31 C32 63.0(4) . . . . ?
C34 Si1 C31 C32 -54.7(5) . . . . ?
C37 Si1 C31 C32 178.7(4) . . . . ?
C2 Si1 C31 C33 -62.2(4) . . . . ?
C34 Si1 C31 C33 -179.9(4) . . . . ?
C37 Si1 C31 C33 53.6(4) . . . . ?
C2 Si1 C34 C35 -32.8(5) . . . . ?
C31 Si1 C34 C35 85.6(5) . . . . ?
C37 Si1 C34 C35 -149.0(4) . . . . ?
C2 Si1 C34 C36 -162.3(4) . . . . ?
C31 Si1 C34 C36 -43.8(5) . . . . ?
C37 Si1 C34 C36 81.5(5) . . . . ?
C2 Si1 C37 C38 -54.1(5) . . . . ?
C34 Si1 C37 C38 62.0(5) . . . . ?
C31 Si1 C37 C38 -170.6(5) . . . . ?
C2 Si1 C37 C39 176.1(4) . . . . ?
C34 Si1 C37 C39 -67.8(4) . . . . ?
C31 Si1 C37 C39 59.7(5) . . . . ?
C3 C4 Si2 C47 -19(3) . . . . ?
Si2B C4 Si2 C47 136(2) . . . . ?
C3 C4 Si2 C41 -143(3) . . . . ?
Si2B C4 Si2 C41 12.0(17) . . . . ?
C3 C4 Si2 C44 101(3) . . . . ?
Si2B C4 Si2 C44 -103(2) . . . . ?
C47 Si2 C41 C43 -56.3(10) . . . . ?
C4 Si2 C41 C43 67.8(9) . . . . ?
C44 Si2 C41 C43 -179.5(9) . . . . ?
C47 Si2 C41 C42 174.4(9) . . . . ?
C4 Si2 C41 C42 -61.6(9) . . . . ?
C44 Si2 C41 C42 51.1(10) . . . . ?
C47 Si2 C44 C46 70.5(16) . . . . ?
C4 Si2 C44 C46 -50.6(16) . . . . ?
C41 Si2 C44 C46 -165.2(15) . . . . ?
C47 Si2 C44 C45 -56.4(17) . . . . ?
C4 Si2 C44 C45 -177.5(17) . . . . ?
C41 Si2 C44 C45 67.8(17) . . . . ?
C4 Si2 C47 C48 -17.6(16) . . . . ?
C41 Si2 C47 C48 103.9(16) . . . . ?
C44 Si2 C47 C48 -134.3(15) . . . . ?
C4 Si2 C47 C49 -162.1(13) . . . . ?
C41 Si2 C47 C49 -40.6(15) . . . . ?
C44 Si2 C47 C49 81.3(14) . . . . ?
C3 C4 Si2B C44B -79(6) . . . . ?
Si2 C4 Si2B C44B 141(2) . . . . ?
C3 C4 Si2B C41B 160(5) . . . . ?
Si2 C4 Si2B C41B 20.2(18) . . . . ?
C3 C4 Si2B C47B 43(6) . . . . ?
Si2 C4 Si2B C47B -96.3(19) . . . . ?
C4 Si2B C41B C42B 58.9(13) . . . . ?
C44B Si2B C41B C42B -62.0(14) . . . . ?
C47B Si2B C41B C42B 168.6(14) . . . . ?
C4 Si2B C41B C43B -174.0(11) . . . . ?
C44B Si2B C41B C43B 65.1(12) . . . . ?
C47B Si2B C41B C43B -64.3(13) . . . . ?
C4 Si2B C44B C45B -88.9(15) . . . . ?
C41B Si2B C44B C45B 25.7(16) . . . . ?
C47B Si2B C44B C45B 154.6(14) . . . . ?
C4 Si2B C44B C46B 40.7(13) . . . . ?
C41B Si2B C44B C46B 155.3(12) . . . . ?
C47B Si2B C44B C46B -75.8(15) . . . . ?
C4 Si2B C47B C48B -72.3(15) . . . . ?
C44B Si2B C47B C48B 49.7(17) . . . . ?
C41B Si2B C47B C48B 178.9(16) . . . . ?
C4 Si2B C47B C49B 56.9(13) . . . . ?
C44B Si2B C47B C49B 178.9(13) . . . . ?
C41B Si2B C47B C49B -51.9(15) . . . . ?
_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full 21.51
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max 0.411
_refine_diff_density_min -0.224
_refine_diff_density_rms 0.043
#==================================================================
data_bli5
_database_code_depnum_ccdc_archive 'CCDC 846083'
#TrackingRef '- BLI BC 2011.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C28 H44 N2 S Si2'
_chemical_formula_weight 496.89
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.3360(14)
_cell_length_b 14.9701(15)
_cell_length_c 14.9722(16)
_cell_angle_alpha 90.00
_cell_angle_beta 97.892(2)
_cell_angle_gamma 90.00
_cell_volume 3182.8(6)
_cell_formula_units_Z 4
_cell_measurement_temperature 200(2)
_cell_measurement_reflns_used 1513
_cell_measurement_theta_min 2.29
_cell_measurement_theta_max 16.55
_exptl_crystal_description polyhedron
_exptl_crystal_colour light_blue
_exptl_crystal_size_max 0.29
_exptl_crystal_size_mid 0.17
_exptl_crystal_size_min 0.14
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.037
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1080
_exptl_absorpt_coefficient_mu 0.194
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.9460
_exptl_absorpt_correction_T_max 0.9734
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 200(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 14129
_diffrn_reflns_av_R_equivalents 0.0491
_diffrn_reflns_av_sigmaI/netI 0.0344
_diffrn_reflns_limit_h_min -13
_diffrn_reflns_limit_h_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_l_min -13
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 1.84
_diffrn_reflns_theta_max 19.25
_reflns_number_total 2647
_reflns_number_gt 1662
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1447P)^2^+1.6184P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 2647
_refine_ls_number_parameters 302
_refine_ls_number_restraints 294
_refine_ls_R_factor_all 0.1112
_refine_ls_R_factor_gt 0.0728
_refine_ls_wR_factor_ref 0.2437
_refine_ls_wR_factor_gt 0.2099
_refine_ls_goodness_of_fit_ref 1.035
_refine_ls_restrained_S_all 1.237
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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 0.2459(2) 1.45536(16) 1.20046(17) 0.1244(12) Uani 1 1 d DU . .
Si2 Si 0.23589(17) 0.77874(14) 0.79664(15) 0.1033(10) Uani 1 1 d DU . .
C1 C 0.2275(6) 1.2822(5) 1.0961(5) 0.112(3) Uani 1 1 d DU . .
C2 C 0.2330(6) 1.3504(5) 1.1375(5) 0.117(3) Uani 1 1 d DU . .
C3 C 0.2294(6) 0.9521(5) 0.8986(5) 0.105(3) Uani 1 1 d DU A .
C4 C 0.2315(5) 0.8837(5) 0.8579(5) 0.107(3) Uani 1 1 d DU . .
C11 C 0.2242(6) 1.1988(4) 1.0461(5) 0.097(2) Uani 1 1 d DU . .
C12 C 0.3101(6) 1.1591(5) 1.0350(5) 0.097(2) Uani 1 1 d DU A .
N13 N 0.3950(5) 1.1869(5) 1.0654(5) 0.133(3) Uani 1 1 d DU . .
S1 S 0.4685(2) 1.11610(19) 1.0364(2) 0.1454(17) Uani 0.877(7) 1 d PDU . .
N14 N 0.3974(5) 1.0458(4) 0.9837(5) 0.127(3) Uani 1 1 d DU . .
C15 C 0.3112(6) 1.0745(5) 0.9854(5) 0.096(2) Uani 1 1 d DU A .
C16 C 0.2261(6) 1.0353(4) 0.9480(5) 0.093(2) Uani 1 1 d DU . .
C17 C 0.1444(6) 1.0753(5) 0.9609(5) 0.107(3) Uani 1 1 d DU A 1
H17 H 0.0863 1.0481 0.9374 0.128 Uiso 1 1 calc R A 1
C18 C 0.1435(6) 1.1589(5) 1.0097(5) 0.113(3) Uani 1 1 d DU A 1
H18 H 0.0849 1.1862 1.0161 0.136 Uiso 1 1 calc R A 1
C31 C 0.3523(8) 1.5117(7) 1.1785(8) 0.288(9) Uani 1 1 d DU . .
H31 H 0.3937 1.4733 1.2220 0.346 Uiso 1 1 calc R . .
C32 C 0.3796(13) 1.5940(11) 1.2292(14) 0.404(17) Uani 1 1 d DU . .
H32A H 0.3420 1.6000 1.2789 0.606 Uiso 1 1 calc R . .
H32B H 0.3683 1.6456 1.1889 0.606 Uiso 1 1 calc R . .
H32C H 0.4465 1.5912 1.2535 0.606 Uiso 1 1 calc R . .
C33 C 0.4008(8) 1.4890(9) 1.1055(8) 0.221(6) Uani 1 1 d DU . .
H33A H 0.3764 1.4324 1.0791 0.332 Uiso 1 1 calc R . .
H33B H 0.4682 1.4829 1.1272 0.332 Uiso 1 1 calc R . .
H33C H 0.3914 1.5361 1.0597 0.332 Uiso 1 1 calc R . .
C34 C 0.2506(6) 1.4268(6) 1.3217(5) 0.160(4) Uani 1 1 d DU . .
H34 H 0.2548 1.4848 1.3551 0.192 Uiso 1 1 calc R . .
C35 C 0.3361(9) 1.3748(9) 1.3581(7) 0.285(8) Uani 1 1 d DU . .
H35A H 0.3925 1.4068 1.3455 0.427 Uiso 1 1 calc R . .
H35B H 0.3338 1.3159 1.3294 0.427 Uiso 1 1 calc R . .
H35C H 0.3382 1.3676 1.4234 0.427 Uiso 1 1 calc R . .
C36 C 0.1631(9) 1.3822(9) 1.3425(7) 0.248(7) Uani 1 1 d DU . .
H36A H 0.1084 1.4192 1.3205 0.372 Uiso 1 1 calc R . .
H36B H 0.1667 1.3742 1.4079 0.372 Uiso 1 1 calc R . .
H36C H 0.1568 1.3237 1.3129 0.372 Uiso 1 1 calc R . .
C37 C 0.1395(8) 1.5234(6) 1.1641(6) 0.213(6) Uani 1 1 d DU . .
H37 H 0.0880 1.4844 1.1809 0.256 Uiso 1 1 calc R . .
C38 C 0.1293(11) 1.6043(8) 1.2177(10) 0.310(11) Uani 1 1 d DU . .
H38A H 0.1493 1.5914 1.2816 0.464 Uiso 1 1 calc R . .
H38B H 0.0633 1.6232 1.2091 0.464 Uiso 1 1 calc R . .
H38C H 0.1685 1.6521 1.1981 0.464 Uiso 1 1 calc R . .
C39 C 0.1131(12) 1.5337(11) 1.0675(8) 0.338(13) Uani 1 1 d DU . .
H39A H 0.1170 1.4757 1.0379 0.507 Uiso 1 1 calc R . .
H39B H 0.1560 1.5760 1.0441 0.507 Uiso 1 1 calc R . .
H39C H 0.0485 1.5563 1.0552 0.507 Uiso 1 1 calc R . .
C41 C 0.1357(6) 0.7095(5) 0.8123 0.232(7) Uani 1 1 d DU . .
H41 H 0.0971 0.7400 0.7603 0.279 Uiso 1 1 calc R . .
C42 C 0.0689(8) 0.7342(9) 0.8692(10) 0.252(8) Uani 1 1 d DU . .
H42A H 0.0837 0.7941 0.8936 0.378 Uiso 1 1 calc R . .
H42B H 0.0710 0.6913 0.9189 0.378 Uiso 1 1 calc R . .
H42C H 0.0057 0.7343 0.8345 0.378 Uiso 1 1 calc R . .
C43 C 0.1243(10) 0.6240(8) 0.7640(13) 0.316(12) Uani 1 1 d DU . .
H43A H 0.1752 0.6167 0.7271 0.473 Uiso 1 1 calc R . .
H43B H 0.0635 0.6232 0.7249 0.473 Uiso 1 1 calc R . .
H43C H 0.1265 0.5750 0.8076 0.473 Uiso 1 1 calc R . .
C44 C 0.3479(6) 0.7227(6) 0.8403(6) 0.180(5) Uani 1 1 d DU . .
H44 H 0.3973 0.7679 0.8317 0.216 Uiso 1 1 calc R . .
C45 C 0.3711(10) 0.6445(9) 0.7854(9) 0.325(12) Uani 1 1 d DU . .
H45A H 0.3607 0.6604 0.7213 0.488 Uiso 1 1 calc R . .
H45B H 0.3306 0.5940 0.7961 0.488 Uiso 1 1 calc R . .
H45C H 0.4372 0.6279 0.8027 0.488 Uiso 1 1 calc R . .
C46 C 0.3628(8) 0.7046(8) 0.9376(6) 0.217(6) Uani 1 1 d DU . .
H46A H 0.3482 0.7584 0.9704 0.325 Uiso 1 1 calc R . .
H46B H 0.4286 0.6876 0.9563 0.325 Uiso 1 1 calc R . .
H46C H 0.3214 0.6557 0.9511 0.325 Uiso 1 1 calc R . .
C47 C 0.2371(6) 0.8075(6) 0.6757(4) 0.159(4) Uani 1 1 d DU . .
H47 H 0.2408 0.7496 0.6431 0.191 Uiso 1 1 calc R . .
C48 C 0.1489(10) 0.8524(10) 0.6337(7) 0.291(8) Uani 1 1 d DU . .
H48A H 0.0946 0.8149 0.6414 0.437 Uiso 1 1 calc R . .
H48B H 0.1515 0.8615 0.5693 0.437 Uiso 1 1 calc R . .
H48C H 0.1428 0.9103 0.6629 0.437 Uiso 1 1 calc R . .
C49 C 0.3224(10) 0.8595(9) 0.6612(7) 0.273(8) Uani 1 1 d DU . .
H49A H 0.3790 0.8270 0.6872 0.410 Uiso 1 1 calc R . .
H49B H 0.3209 0.9180 0.6904 0.410 Uiso 1 1 calc R . .
H49C H 0.3233 0.8678 0.5964 0.410 Uiso 1 1 calc R . .
S1B S 0.033(2) 1.121(2) 0.992(2) 0.211(17) Uiso 0.123(7) 1 d P B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.181(3) 0.0863(18) 0.112(2) -0.0356(14) 0.0429(18) -0.0151(16)
Si2 0.139(2) 0.0750(16) 0.0984(19) -0.0247(12) 0.0230(14) -0.0050(13)
C1 0.185(9) 0.071(5) 0.087(6) -0.013(4) 0.035(5) 0.000(5)
C2 0.177(8) 0.075(5) 0.104(6) -0.019(4) 0.035(6) -0.004(5)
C3 0.162(8) 0.070(5) 0.087(6) -0.010(4) 0.030(5) -0.005(5)
C4 0.161(8) 0.076(5) 0.086(5) -0.014(4) 0.023(5) -0.007(5)
C11 0.151(7) 0.073(5) 0.072(5) 0.001(4) 0.030(5) 0.010(5)
C12 0.131(6) 0.077(5) 0.083(5) 0.000(4) 0.016(5) -0.005(5)
N13 0.141(6) 0.107(5) 0.151(7) -0.026(5) 0.021(5) -0.007(5)
S1 0.128(3) 0.110(2) 0.200(4) -0.056(2) 0.029(2) -0.0083(17)
N14 0.135(5) 0.106(5) 0.143(6) -0.031(4) 0.026(5) -0.002(4)
C15 0.134(6) 0.068(5) 0.089(6) 0.003(4) 0.024(5) 0.007(4)
C16 0.135(6) 0.073(5) 0.073(5) -0.003(4) 0.016(5) -0.006(4)
C17 0.140(6) 0.081(5) 0.104(6) -0.014(4) 0.029(5) 0.006(5)
C18 0.142(7) 0.089(6) 0.108(7) -0.019(5) 0.019(6) -0.007(5)
C31 0.336(14) 0.255(15) 0.319(19) -0.169(13) 0.208(15) -0.178(13)
C32 0.42(3) 0.31(2) 0.53(3) -0.28(2) 0.25(2) -0.25(2)
C33 0.239(14) 0.231(14) 0.213(14) -0.033(11) 0.101(11) -0.042(11)
C34 0.245(12) 0.130(9) 0.105(6) -0.038(5) 0.029(7) 0.006(7)
C35 0.394(17) 0.253(17) 0.180(12) -0.044(12) -0.058(14) 0.124(14)
C36 0.387(16) 0.215(14) 0.163(11) -0.019(10) 0.115(12) -0.091(13)
C37 0.325(13) 0.127(9) 0.182(10) -0.030(8) 0.015(11) 0.086(9)
C38 0.37(2) 0.204(15) 0.330(19) -0.138(14) -0.032(17) 0.115(14)
C39 0.44(3) 0.32(2) 0.214(12) -0.036(15) -0.089(17) 0.13(2)
C41 0.253(11) 0.173(11) 0.302(17) -0.122(10) 0.150(12) -0.105(10)
C42 0.271(16) 0.227(15) 0.292(18) -0.079(13) 0.165(14) -0.088(12)
C43 0.271(17) 0.188(13) 0.52(3) -0.197(16) 0.174(18) -0.119(12)
C44 0.223(9) 0.148(9) 0.159(8) -0.046(7) -0.012(9) 0.065(8)
C45 0.300(19) 0.293(19) 0.349(18) -0.187(17) -0.078(16) 0.171(15)
C46 0.259(15) 0.178(11) 0.189(10) 0.023(9) -0.053(11) 0.010(10)
C47 0.257(13) 0.121(8) 0.103(6) -0.035(5) 0.031(7) 0.014(7)
C48 0.449(18) 0.269(17) 0.135(10) -0.005(11) -0.038(13) 0.173(15)
C49 0.468(19) 0.201(14) 0.185(13) -0.043(11) 0.164(14) -0.141(14)
_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 C31 1.812(7) . ?
Si1 C2 1.828(7) . ?
Si1 C37 1.852(8) . ?
Si1 C34 1.857(7) . ?
Si2 C41 1.813(7) . ?
Si2 C4 1.824(7) . ?
Si2 C44 1.850(7) . ?
Si2 C47 1.864(7) . ?
C1 C2 1.192(8) . ?
C1 C11 1.452(9) . ?
C3 C4 1.195(7) . ?
C3 C16 1.453(9) . ?
C11 C18 1.349(9) . ?
C11 C12 1.399(8) . ?
C12 N13 1.307(8) . ?
C12 C15 1.469(11) . ?
N13 S1 1.596(7) . ?
S1 N14 1.596(7) . ?
N14 C15 1.311(8) . ?
C15 C16 1.400(8) . ?
C16 C17 1.352(8) . ?
C17 C18 1.451(11) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C31 C33 1.415(7) . ?
C31 C32 1.471(8) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.491(8) . ?
C34 C35 1.491(8) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.452(8) . ?
C37 C38 1.471(8) . ?
C37 H37 1.0000 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C41 C42 1.415(7) . ?
C41 C43 1.469(7) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C46 1.468(8) . ?
C44 C45 1.494(8) . ?
C44 H44 1.0000 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C49 1.490(8) . ?
C47 C48 1.493(8) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
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
C31 Si1 C2 109.5(3) . . ?
C31 Si1 C37 111.7(4) . . ?
C2 Si1 C37 107.5(4) . . ?
C31 Si1 C34 111.5(4) . . ?
C2 Si1 C34 107.1(3) . . ?
C37 Si1 C34 109.4(4) . . ?
C41 Si2 C4 110.2(3) . . ?
C41 Si2 C44 111.1(4) . . ?
C4 Si2 C44 107.5(3) . . ?
C41 Si2 C47 111.8(3) . . ?
C4 Si2 C47 107.1(3) . . ?
C44 Si2 C47 108.9(4) . . ?
C2 C1 C11 178.2(9) . . ?
C1 C2 Si1 177.9(8) . . ?
C4 C3 C16 179.6(9) . . ?
C3 C4 Si2 179.4(8) . . ?
C18 C11 C12 119.0(6) . . ?
C18 C11 C1 123.7(7) . . ?
C12 C11 C1 117.3(7) . . ?
N13 C12 C11 128.0(7) . . ?
N13 C12 C15 112.2(5) . . ?
C11 C12 C15 119.8(5) . . ?
C12 N13 S1 108.1(5) . . ?
N14 S1 N13 99.9(4) . . ?
C15 N14 S1 108.3(5) . . ?
N14 C15 C16 128.8(7) . . ?
N14 C15 C12 111.5(5) . . ?
C16 C15 C12 119.6(5) . . ?
C17 C16 C15 118.8(6) . . ?
C17 C16 C3 122.8(7) . . ?
C15 C16 C3 118.4(7) . . ?
C16 C17 C18 121.4(6) . . ?
C16 C17 H17 119.3 . . ?
C18 C17 H17 119.3 . . ?
C11 C18 C17 121.3(6) . . ?
C11 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C33 C31 C32 118.3(8) . . ?
C33 C31 Si1 123.0(6) . . ?
C32 C31 Si1 117.8(6) . . ?
C33 C31 H31 93.1 . . ?
C32 C31 H31 93.1 . . ?
Si1 C31 H31 93.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C36 C34 C35 111.3(8) . . ?
C36 C34 Si1 112.9(6) . . ?
C35 C34 Si1 113.2(6) . . ?
C36 C34 H34 106.3 . . ?
C35 C34 H34 106.3 . . ?
Si1 C34 H34 106.3 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C39 C37 C38 115.1(8) . . ?
C39 C37 Si1 116.3(7) . . ?
C38 C37 Si1 115.6(7) . . ?
C39 C37 H37 102.2 . . ?
C38 C37 H37 102.2 . . ?
Si1 C37 H37 102.2 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C42 C41 C43 119.0(7) . . ?
C42 C41 Si2 122.9(6) . . ?
C43 C41 Si2 118.1(6) . . ?
C42 C41 H41 90.1 . . ?
C43 C41 H41 90.1 . . ?
Si2 C41 H41 90.1 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C46 C44 C45 112.9(8) . . ?
C46 C44 Si2 115.8(6) . . ?
C45 C44 Si2 114.1(6) . . ?
C46 C44 H44 104.1 . . ?
C45 C44 H44 104.1 . . ?
Si2 C44 H44 104.1 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C49 C47 C48 111.6(8) . . ?
C49 C47 Si2 112.3(5) . . ?
C48 C47 Si2 113.1(6) . . ?
C49 C47 H47 106.4 . . ?
C48 C47 H47 106.4 . . ?
Si2 C47 H47 106.4 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
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
C11 C1 C2 Si1 16(44) . . . . ?
C31 Si1 C2 C1 17(21) . . . . ?
C37 Si1 C2 C1 139(21) . . . . ?
C34 Si1 C2 C1 -104(21) . . . . ?
C16 C3 C4 Si2 -136(99) . . . . ?
C41 Si2 C4 C3 109(84) . . . . ?
C44 Si2 C4 C3 -12(84) . . . . ?
C47 Si2 C4 C3 -129(84) . . . . ?
C2 C1 C11 C18 179(100) . . . . ?
C2 C1 C11 C12 -1(26) . . . . ?
C18 C11 C12 N13 -179.6(9) . . . . ?
C1 C11 C12 N13 1.1(13) . . . . ?
C18 C11 C12 C15 -1.0(11) . . . . ?
C1 C11 C12 C15 179.7(7) . . . . ?
C11 C12 N13 S1 178.4(7) . . . . ?
C15 C12 N13 S1 -0.3(9) . . . . ?
C12 N13 S1 N14 0.0(7) . . . . ?
N13 S1 N14 C15 0.3(7) . . . . ?
S1 N14 C15 C16 179.8(7) . . . . ?
S1 N14 C15 C12 -0.5(9) . . . . ?
N13 C12 C15 N14 0.5(10) . . . . ?
C11 C12 C15 N14 -178.3(7) . . . . ?
N13 C12 C15 C16 -179.8(7) . . . . ?
C11 C12 C15 C16 1.4(11) . . . . ?
N14 C15 C16 C17 177.6(8) . . . . ?
C12 C15 C16 C17 -2.0(11) . . . . ?
N14 C15 C16 C3 -1.0(13) . . . . ?
C12 C15 C16 C3 179.4(7) . . . . ?
C4 C3 C16 C17 -4(100) . . . . ?
C4 C3 C16 C15 174(100) . . . . ?
C15 C16 C17 C18 2.1(12) . . . . ?
C3 C16 C17 C18 -179.3(7) . . . . ?
C12 C11 C18 C17 1.1(12) . . . . ?
C1 C11 C18 C17 -179.6(7) . . . . ?
C16 C17 C18 C11 -1.7(12) . . . . ?
C2 Si1 C31 C33 16.0(14) . . . . ?
C37 Si1 C31 C33 -103.0(13) . . . . ?
C34 Si1 C31 C33 134.3(12) . . . . ?
C2 Si1 C31 C32 -174.9(15) . . . . ?
C37 Si1 C31 C32 66.1(16) . . . . ?
C34 Si1 C31 C32 -56.6(16) . . . . ?
C31 Si1 C34 C36 178.7(8) . . . . ?
C2 Si1 C34 C36 -61.5(8) . . . . ?
C37 Si1 C34 C36 54.7(9) . . . . ?
C31 Si1 C34 C35 -53.7(9) . . . . ?
C2 Si1 C34 C35 66.1(8) . . . . ?
C37 Si1 C34 C35 -177.8(8) . . . . ?
C31 Si1 C37 C39 70.2(13) . . . . ?
C2 Si1 C37 C39 -50.0(13) . . . . ?
C34 Si1 C37 C39 -165.9(12) . . . . ?
C31 Si1 C37 C38 -69.4(11) . . . . ?
C2 Si1 C37 C38 170.4(10) . . . . ?
C34 Si1 C37 C38 54.5(11) . . . . ?
C4 Si2 C41 C42 -3.6(10) . . . . ?
C44 Si2 C41 C42 115.4(11) . . . . ?
C47 Si2 C41 C42 -122.6(10) . . . . ?
C4 Si2 C41 C43 176.8(11) . . . . ?
C44 Si2 C41 C43 -64.2(11) . . . . ?
C47 Si2 C41 C43 57.8(12) . . . . ?
C41 Si2 C44 C46 -63.0(8) . . . . ?
C4 Si2 C44 C46 57.6(9) . . . . ?
C47 Si2 C44 C46 173.4(8) . . . . ?
C41 Si2 C44 C45 70.5(10) . . . . ?
C4 Si2 C44 C45 -168.9(10) . . . . ?
C47 Si2 C44 C45 -53.1(11) . . . . ?
C41 Si2 C47 C49 -176.4(8) . . . . ?
C4 Si2 C47 C49 62.9(8) . . . . ?
C44 Si2 C47 C49 -53.1(8) . . . . ?
C41 Si2 C47 C48 56.2(9) . . . . ?
C4 Si2 C47 C48 -64.6(8) . . . . ?
C44 Si2 C47 C48 179.4(8) . . . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full 19.25
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max 0.254
_refine_diff_density_min -0.221
_refine_diff_density_rms 0.043
#==================================================================
data_bli2
_database_code_depnum_ccdc_archive 'CCDC 846084'
#TrackingRef '- BLI BC 2011.cif'
_audit_creation_method SHELXL-97
_chemical_name_systematic
;
?
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety ?
_chemical_formula_sum 'C28 H44 N2 Se Si2'
_chemical_formula_weight 543.79
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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Se Se -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_H-M P2(1)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a 14.751(3)
_cell_length_b 14.938(3)
_cell_length_c 15.035(3)
_cell_angle_alpha 90.00
_cell_angle_beta 105.604(5)
_cell_angle_gamma 90.00
_cell_volume 3190.8(12)
_cell_formula_units_Z 4
_cell_measurement_temperature 200(2)
_cell_measurement_reflns_used 2102
_cell_measurement_theta_min 2.19
_cell_measurement_theta_max 16.04
_exptl_crystal_description polyhedron
_exptl_crystal_colour yellow
_exptl_crystal_size_max 0.22
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.12
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.132
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1152
_exptl_absorpt_coefficient_mu 1.268
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.7677
_exptl_absorpt_correction_T_max 0.8627
_exptl_absorpt_process_details
;
Sheldrick, G. M. (2008). SADABS. University of G\"ottingen, Germany.
;
_exptl_special_details
;
?
;
_diffrn_ambient_temperature 200(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker APEX'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number 16265
_diffrn_reflns_av_R_equivalents 0.0514
_diffrn_reflns_av_sigmaI/netI 0.0396
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 14
_diffrn_reflns_limit_k_min -14
_diffrn_reflns_limit_k_max 14
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.72
_diffrn_reflns_theta_max 20.39
_reflns_number_total 3148
_reflns_number_gt 2306
_reflns_threshold_expression >2sigma(I)
_computing_data_collection 'Bruker APEX'
_computing_cell_refinement 'Bruker SAINT'
_computing_data_reduction 'Bruker SAINT'
_computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics 'Bruker SHELXTL'
_computing_publication_material 'Bruker SHELXTL'
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0614P)^2^+2.6035P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 3148
_refine_ls_number_parameters 298
_refine_ls_number_restraints 262
_refine_ls_R_factor_all 0.0711
_refine_ls_R_factor_gt 0.0485
_refine_ls_wR_factor_ref 0.1348
_refine_ls_wR_factor_gt 0.1217
_refine_ls_goodness_of_fit_ref 1.050
_refine_ls_restrained_S_all 1.183
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
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
Se1 Se -0.00925(6) 0.10690(5) 0.06415(6) 0.1007(4) Uani 1 1 d U . .
Si2 Si -0.24392(16) 0.44500(13) 0.20518(14) 0.0968(7) Uani 1 1 d DU . .
C1 C -0.2663(4) -0.0556(4) -0.1041(4) 0.0758(17) Uani 1 1 d U . .
C2 C -0.2679(5) -0.1243(4) -0.1446(4) 0.0844(19) Uani 1 1 d U . .
C3 C -0.2633(5) 0.2710(4) 0.0983(4) 0.0832(19) Uani 1 1 d U . .
C4 C -0.2579(5) 0.3392(5) 0.1407(5) 0.090(2) Uani 1 1 d U . .
C11 C -0.2651(5) 0.0255(4) -0.0533(4) 0.0701(16) Uani 1 1 d U . .
C12 C -0.1779(5) 0.0657(4) -0.0054(4) 0.0676(15) Uani 1 1 d U . .
N13 N -0.0949(4) 0.0326(3) -0.0038(3) 0.0796(14) Uani 1 1 d U . .
N14 N -0.0943(4) 0.1820(3) 0.0863(4) 0.0898(16) Uani 1 1 d U . .
C15 C -0.1784(5) 0.1488(4) 0.0446(4) 0.0714(16) Uani 1 1 d U . .
C16 C -0.2653(5) 0.1891(4) 0.0479(4) 0.0740(17) Uani 1 1 d U . .
C17 C -0.3458(5) 0.1480(4) 0.0015(5) 0.0876(19) Uani 1 1 d U . .
H17 H -0.4043 0.1739 0.0026 0.105 Uiso 1 1 calc R . .
C18 C -0.3461(5) 0.0672(4) -0.0489(4) 0.0836(18) Uani 1 1 d U . .
H18 H -0.4047 0.0415 -0.0805 0.100 Uiso 1 1 calc R . .
Si1 Si -0.27238(15) -0.23172(12) -0.20730(14) 0.0921(7) Uani 1 1 d DU . .
C41 C -0.1654(7) -0.2949(5) -0.1470(6) 0.145(3) Uani 1 1 d DU . .
H41 H -0.1126 -0.2562 -0.1544 0.174 Uiso 1 1 calc R . .
C42 C -0.1524(10) -0.3814(7) -0.1947(10) 0.283(9) Uani 1 1 d DU . .
H42A H -0.1648 -0.3708 -0.2612 0.425 Uiso 1 1 calc R . .
H42B H -0.1963 -0.4265 -0.1836 0.425 Uiso 1 1 calc R . .
H42C H -0.0877 -0.4027 -0.1700 0.425 Uiso 1 1 calc R . .
C43 C -0.1465(9) -0.3053(7) -0.0473(7) 0.203(5) Uani 1 1 d DU . .
H43A H -0.1537 -0.2474 -0.0193 0.305 Uiso 1 1 calc R . .
H43B H -0.0820 -0.3271 -0.0219 0.305 Uiso 1 1 calc R . .
H43C H -0.1909 -0.3484 -0.0335 0.305 Uiso 1 1 calc R . .
C44 C -0.2658(7) -0.2047(6) -0.3281(5) 0.147(3) Uani 1 1 d DU . .
H44 H -0.2661 -0.2630 -0.3609 0.177 Uiso 1 1 calc R . .
C45 C -0.1753(10) -0.1580(9) -0.3273(8) 0.243(6) Uani 1 1 d DU . .
H45A H -0.1219 -0.1948 -0.2941 0.365 Uiso 1 1 calc R . .
H45B H -0.1728 -0.1000 -0.2964 0.365 Uiso 1 1 calc R . .
H45C H -0.1720 -0.1488 -0.3909 0.365 Uiso 1 1 calc R . .
C46 C -0.3516(11) -0.1527(9) -0.3814(7) 0.273(7) Uani 1 1 d DU . .
H46A H -0.4087 -0.1865 -0.3820 0.410 Uiso 1 1 calc R . .
H46B H -0.3482 -0.1434 -0.4450 0.410 Uiso 1 1 calc R . .
H46C H -0.3533 -0.0946 -0.3517 0.410 Uiso 1 1 calc R . .
C47 C -0.3836(7) -0.2871(7) -0.2093(9) 0.220(6) Uani 1 1 d DU . .
H47 H -0.4254 -0.2481 -0.2572 0.264 Uiso 1 1 calc R . .
C48 C -0.4303(8) -0.2751(7) -0.1409(8) 0.181(4) Uani 1 1 d DU . .
H48A H -0.4187 -0.2144 -0.1158 0.271 Uiso 1 1 calc R . .
H48B H -0.4070 -0.3187 -0.0913 0.271 Uiso 1 1 calc R . .
H48C H -0.4980 -0.2838 -0.1675 0.271 Uiso 1 1 calc R . .
C49 C -0.4021(9) -0.3741(8) -0.2636(12) 0.299(10) Uani 1 1 d DU . .
H49A H -0.3658 -0.3747 -0.3095 0.449 Uiso 1 1 calc R . .
H49B H -0.4693 -0.3788 -0.2951 0.449 Uiso 1 1 calc R . .
H49C H -0.3831 -0.4248 -0.2213 0.449 Uiso 1 1 calc R . .
C51 C -0.1379(9) 0.5014(8) 0.1912(9) 0.232(6) Uani 1 1 d DU . .
H51 H -0.0957 0.4611 0.2374 0.279 Uiso 1 1 calc R . .
C52 C -0.1072(11) 0.5826(9) 0.2517(12) 0.307(11) Uani 1 1 d DU . .
H52A H -0.1480 0.5898 0.2930 0.461 Uiso 1 1 calc R . .
H52B H -0.1117 0.6360 0.2129 0.461 Uiso 1 1 calc R . .
H52C H -0.0419 0.5747 0.2885 0.461 Uiso 1 1 calc R . .
C53 C -0.0928(9) 0.4829(10) 0.1277(10) 0.252(7) Uani 1 1 d DU . .
H53A H -0.1213 0.4303 0.0921 0.379 Uiso 1 1 calc R . .
H53B H -0.0264 0.4706 0.1581 0.379 Uiso 1 1 calc R . .
H53C H -0.0974 0.5342 0.0861 0.379 Uiso 1 1 calc R . .
C54 C -0.3560(8) 0.5093(6) 0.1537(6) 0.169(4) Uani 1 1 d DU . .
H54 H -0.4073 0.4664 0.1562 0.203 Uiso 1 1 calc R . .
C55 C -0.3724(11) 0.5870(8) 0.2080(10) 0.286(9) Uani 1 1 d DU . .
H55A H -0.3602 0.5698 0.2730 0.429 Uiso 1 1 calc R . .
H55B H -0.4378 0.6069 0.1847 0.429 Uiso 1 1 calc R . .
H55C H -0.3300 0.6359 0.2022 0.429 Uiso 1 1 calc R . .
C56 C -0.3736(11) 0.5305(10) 0.0547(8) 0.275(8) Uani 1 1 d DU . .
H56A H -0.3642 0.4766 0.0211 0.413 Uiso 1 1 calc R . .
H56B H -0.3298 0.5772 0.0467 0.413 Uiso 1 1 calc R . .
H56C H -0.4384 0.5517 0.0305 0.413 Uiso 1 1 calc R . .
C57 C -0.2340(6) 0.4176(6) 0.3282(5) 0.123(3) Uani 1 1 d DU . .
H57 H -0.2306 0.4758 0.3618 0.147 Uiso 1 1 calc R . .
C58 C -0.1466(8) 0.3663(8) 0.3744(7) 0.209(5) Uani 1 1 d DU . .
H58A H -0.0912 0.3995 0.3685 0.314 Uiso 1 1 calc R . .
H58B H -0.1484 0.3076 0.3448 0.314 Uiso 1 1 calc R . .
H58C H -0.1432 0.3582 0.4399 0.314 Uiso 1 1 calc R . .
C59 C -0.3193(8) 0.3691(8) 0.3396(7) 0.190(5) Uani 1 1 d DU . .
H59A H -0.3758 0.4045 0.3118 0.286 Uiso 1 1 calc R . .
H59B H -0.3137 0.3604 0.4054 0.286 Uiso 1 1 calc R . .
H59C H -0.3242 0.3107 0.3089 0.286 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Se1 0.1026(6) 0.0779(5) 0.1209(7) -0.0352(4) 0.0290(5) -0.0126(4)
Si2 0.1349(18) 0.0647(12) 0.1002(15) -0.0269(11) 0.0477(13) -0.0088(12)
C1 0.099(5) 0.059(4) 0.067(4) -0.010(3) 0.019(3) -0.006(3)
C2 0.112(5) 0.063(4) 0.076(4) -0.016(3) 0.022(4) -0.009(4)
C3 0.116(5) 0.060(4) 0.077(5) -0.006(3) 0.032(4) 0.001(4)
C4 0.124(6) 0.069(4) 0.080(5) -0.015(3) 0.035(4) 0.002(4)
C11 0.101(4) 0.045(3) 0.064(4) 0.001(3) 0.021(4) -0.004(3)
C12 0.100(4) 0.043(3) 0.062(4) -0.003(3) 0.026(3) -0.006(3)
N13 0.096(4) 0.058(3) 0.083(4) -0.015(3) 0.020(3) -0.006(3)
N14 0.106(4) 0.063(3) 0.101(4) -0.026(3) 0.029(3) -0.007(3)
C15 0.105(4) 0.046(3) 0.063(4) -0.003(3) 0.023(4) -0.005(3)
C16 0.103(5) 0.048(3) 0.073(4) -0.005(3) 0.027(4) 0.002(3)
C17 0.104(5) 0.066(4) 0.091(5) -0.006(4) 0.023(4) 0.012(4)
C18 0.096(5) 0.067(4) 0.079(5) -0.014(3) 0.008(4) -0.002(4)
Si1 0.1146(16) 0.0635(12) 0.0939(15) -0.0285(10) 0.0205(12) -0.0064(11)
C41 0.180(7) 0.091(6) 0.143(6) -0.034(5) 0.006(6) 0.025(5)
C42 0.270(16) 0.168(11) 0.326(15) -0.127(11) -0.068(13) 0.117(10)
C43 0.271(14) 0.139(9) 0.159(7) 0.043(7) -0.012(9) 0.016(9)
C44 0.235(10) 0.107(7) 0.095(5) -0.045(5) 0.038(6) 0.012(6)
C45 0.410(15) 0.205(12) 0.168(10) -0.073(9) 0.170(11) -0.141(12)
C46 0.445(17) 0.189(12) 0.123(8) 0.005(8) -0.030(12) 0.121(13)
C47 0.180(8) 0.210(11) 0.313(15) -0.193(11) 0.142(10) -0.103(8)
C48 0.198(10) 0.155(9) 0.215(11) -0.049(8) 0.101(8) -0.071(8)
C49 0.218(13) 0.226(14) 0.50(3) -0.260(16) 0.177(15) -0.135(11)
C51 0.283(11) 0.195(11) 0.290(15) -0.136(10) 0.200(12) -0.145(10)
C52 0.36(2) 0.204(13) 0.44(2) -0.185(14) 0.236(19) -0.198(14)
C53 0.237(14) 0.268(16) 0.317(18) -0.090(13) 0.186(13) -0.087(12)
C54 0.256(9) 0.108(7) 0.136(7) -0.007(6) 0.041(7) 0.083(7)
C55 0.321(18) 0.209(13) 0.285(14) -0.105(12) 0.007(14) 0.143(13)
C56 0.35(2) 0.277(18) 0.161(8) 0.053(10) 0.011(11) 0.112(15)
C57 0.158(7) 0.115(6) 0.091(5) -0.029(4) 0.026(5) -0.005(5)
C58 0.249(10) 0.197(12) 0.143(9) 0.006(8) -0.016(9) 0.059(9)
C59 0.267(11) 0.199(11) 0.128(8) -0.016(7) 0.093(8) -0.082(9)
_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
Se1 N14 1.780(5) . ?
Se1 N13 1.783(5) . ?
Si2 C4 1.837(7) . ?
Si2 C51 1.837(9) . ?
Si2 C57 1.861(7) . ?
Si2 C54 1.889(8) . ?
C1 C2 1.190(8) . ?
C1 C11 1.430(8) . ?
C2 Si1 1.853(6) . ?
C3 C4 1.192(8) . ?
C3 C16 1.436(9) . ?
C11 C18 1.364(8) . ?
C11 C12 1.427(8) . ?
C12 N13 1.315(7) . ?
C12 C15 1.453(8) . ?
N14 C15 1.326(7) . ?
C15 C16 1.429(8) . ?
C16 C17 1.352(8) . ?
C17 C18 1.424(9) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
Si1 C47 1.831(8) . ?
Si1 C41 1.852(8) . ?
Si1 C44 1.889(8) . ?
C41 C43 1.457(10) . ?
C41 C42 1.515(9) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.504(11) . ?
C44 C46 1.517(11) . ?
C44 H44 1.0000 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.395(10) . ?
C47 C49 1.519(10) . ?
C47 H47 1.0000 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C51 C53 1.332(10) . ?
C51 C52 1.511(10) . ?
C51 H51 1.0000 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 C56 1.474(10) . ?
C54 C55 1.475(10) . ?
C54 H54 1.0000 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C58 1.499(10) . ?
C57 C59 1.502(10) . ?
C57 H57 1.0000 . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
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
N14 Se1 N13 94.2(3) . . ?
C4 Si2 C51 108.2(4) . . ?
C4 Si2 C57 107.6(3) . . ?
C51 Si2 C57 111.9(5) . . ?
C4 Si2 C54 105.1(4) . . ?
C51 Si2 C54 113.4(6) . . ?
C57 Si2 C54 110.2(4) . . ?
C2 C1 C11 178.3(7) . . ?
C1 C2 Si1 179.0(7) . . ?
C4 C3 C16 177.4(8) . . ?
C3 C4 Si2 177.2(7) . . ?
C18 C11 C12 117.7(6) . . ?
C18 C11 C1 121.9(6) . . ?
C12 C11 C1 120.4(6) . . ?
N13 C12 C11 124.1(5) . . ?
N13 C12 C15 116.5(6) . . ?
C11 C12 C15 119.5(6) . . ?
C12 N13 Se1 106.8(4) . . ?
C15 N14 Se1 107.0(4) . . ?
N14 C15 C16 124.0(5) . . ?
N14 C15 C12 115.5(6) . . ?
C16 C15 C12 120.4(6) . . ?
C17 C16 C15 117.6(6) . . ?
C17 C16 C3 123.3(6) . . ?
C15 C16 C3 119.1(6) . . ?
C16 C17 C18 122.4(6) . . ?
C16 C17 H17 118.8 . . ?
C18 C17 H17 118.8 . . ?
C11 C18 C17 122.4(6) . . ?
C11 C18 H18 118.8 . . ?
C17 C18 H18 118.8 . . ?
C47 Si1 C41 114.8(6) . . ?
C47 Si1 C2 108.0(4) . . ?
C41 Si1 C2 106.4(3) . . ?
C47 Si1 C44 111.0(5) . . ?
C41 Si1 C44 108.8(4) . . ?
C2 Si1 C44 107.5(3) . . ?
C43 C41 C42 112.5(9) . . ?
C43 C41 Si1 117.4(7) . . ?
C42 C41 Si1 113.7(7) . . ?
C43 C41 H41 103.7 . . ?
C42 C41 H41 103.7 . . ?
Si1 C41 H41 103.7 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C45 C44 C46 112.3(10) . . ?
C45 C44 Si1 111.5(7) . . ?
C46 C44 Si1 111.5(7) . . ?
C45 C44 H44 107.1 . . ?
C46 C44 H44 107.1 . . ?
Si1 C44 H44 107.1 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C48 C47 C49 117.0(9) . . ?
C48 C47 Si1 123.2(7) . . ?
C49 C47 Si1 115.2(7) . . ?
C48 C47 H47 97.2 . . ?
C49 C47 H47 97.2 . . ?
Si1 C47 H47 97.2 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C47 C49 H49A 109.5 . . ?
C47 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C47 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C53 C51 C52 118.1(10) . . ?
C53 C51 Si2 126.3(8) . . ?
C52 C51 Si2 115.2(7) . . ?
C53 C51 H51 92.0 . . ?
C52 C51 H51 92.0 . . ?
Si2 C51 H51 92.0 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C56 C54 C55 112.3(9) . . ?
C56 C54 Si2 114.8(8) . . ?
C55 C54 Si2 115.4(8) . . ?
C56 C54 H54 104.2 . . ?
C55 C54 H54 104.2 . . ?
Si2 C54 H54 104.2 . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C58 C57 C59 110.1(9) . . ?
C58 C57 Si2 113.6(7) . . ?
C59 C57 Si2 112.0(6) . . ?
C58 C57 H57 106.9 . . ?
C59 C57 H57 106.9 . . ?
Si2 C57 H57 106.9 . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C57 C59 H59A 109.5 . . ?
C57 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C57 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
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
C11 C1 C2 Si1 49(56) . . . . ?
C16 C3 C4 Si2 17(27) . . . . ?
C51 Si2 C4 C3 9(14) . . . . ?
C57 Si2 C4 C3 -112(14) . . . . ?
C54 Si2 C4 C3 131(14) . . . . ?
C2 C1 C11 C18 -75(26) . . . . ?
C2 C1 C11 C12 106(26) . . . . ?
C18 C11 C12 N13 179.8(6) . . . . ?
C1 C11 C12 N13 -0.3(9) . . . . ?
C18 C11 C12 C15 -0.8(8) . . . . ?
C1 C11 C12 C15 179.1(5) . . . . ?
C11 C12 N13 Se1 179.7(4) . . . . ?
C15 C12 N13 Se1 0.3(6) . . . . ?
N14 Se1 N13 C12 -0.6(4) . . . . ?
N13 Se1 N14 C15 0.7(4) . . . . ?
Se1 N14 C15 C16 178.6(5) . . . . ?
Se1 N14 C15 C12 -0.6(6) . . . . ?
N13 C12 C15 N14 0.2(8) . . . . ?
C11 C12 C15 N14 -179.2(5) . . . . ?
N13 C12 C15 C16 -179.1(5) . . . . ?
C11 C12 C15 C16 1.5(8) . . . . ?
N14 C15 C16 C17 179.5(6) . . . . ?
C12 C15 C16 C17 -1.2(9) . . . . ?
N14 C15 C16 C3 0.5(9) . . . . ?
C12 C15 C16 C3 179.7(5) . . . . ?
C4 C3 C16 C17 -173(15) . . . . ?
C4 C3 C16 C15 6(15) . . . . ?
C15 C16 C17 C18 0.3(9) . . . . ?
C3 C16 C17 C18 179.3(6) . . . . ?
C12 C11 C18 C17 -0.2(9) . . . . ?
C1 C11 C18 C17 180.0(6) . . . . ?
C16 C17 C18 C11 0.4(10) . . . . ?
C1 C2 Si1 C47 -1(39) . . . . ?
C1 C2 Si1 C41 -124(39) . . . . ?
C1 C2 Si1 C44 119(39) . . . . ?
C47 Si1 C41 C43 -68.1(9) . . . . ?
C2 Si1 C41 C43 51.4(9) . . . . ?
C44 Si1 C41 C43 166.9(8) . . . . ?
C47 Si1 C41 C42 66.2(11) . . . . ?
C2 Si1 C41 C42 -174.4(9) . . . . ?
C44 Si1 C41 C42 -58.8(11) . . . . ?
C47 Si1 C44 C45 179.2(8) . . . . ?
C41 Si1 C44 C45 -53.5(8) . . . . ?
C2 Si1 C44 C45 61.3(8) . . . . ?
C47 Si1 C44 C46 52.9(9) . . . . ?
C41 Si1 C44 C46 -179.9(8) . . . . ?
C2 Si1 C44 C46 -65.1(8) . . . . ?
C41 Si1 C47 C48 89.9(13) . . . . ?
C2 Si1 C47 C48 -28.6(14) . . . . ?
C44 Si1 C47 C48 -146.2(12) . . . . ?
C41 Si1 C47 C49 -65.2(13) . . . . ?
C2 Si1 C47 C49 176.3(11) . . . . ?
C44 Si1 C47 C49 58.7(13) . . . . ?
C4 Si2 C51 C53 16.2(18) . . . . ?
C57 Si2 C51 C53 134.6(16) . . . . ?
C54 Si2 C51 C53 -99.9(17) . . . . ?
C4 Si2 C51 C52 -170.9(12) . . . . ?
C57 Si2 C51 C52 -52.5(14) . . . . ?
C54 Si2 C51 C52 73.0(14) . . . . ?
C4 Si2 C54 C56 -61.2(10) . . . . ?
C51 Si2 C54 C56 56.7(11) . . . . ?
C57 Si2 C54 C56 -176.9(9) . . . . ?
C4 Si2 C54 C55 165.8(10) . . . . ?
C51 Si2 C54 C55 -76.3(11) . . . . ?
C57 Si2 C54 C55 50.1(11) . . . . ?
C4 Si2 C57 C58 65.9(8) . . . . ?
C51 Si2 C57 C58 -52.9(9) . . . . ?
C54 Si2 C57 C58 179.9(8) . . . . ?
C4 Si2 C57 C59 -59.6(8) . . . . ?
C51 Si2 C57 C59 -178.3(8) . . . . ?
C54 Si2 C57 C59 54.5(8) . . . . ?
_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full 20.39
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max 0.279
_refine_diff_density_min -0.196
_refine_diff_density_rms 0.043
#==================================================================