#------------------------------------------------------------------------------
#$Date: 2016-03-21 05:33:32 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178484 $
#$URL: svn://www.crystallography.net/cod/cif/4/03/05/4030572.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_4030572
loop_
_publ_author_name
'Hammer, Natalie'
'Shubina, Tatyana E.'
'Gisselbrecht, Jean-Paul'
'Hampel, Frank'
'Kivala, Milan'
_publ_section_title
;
 Synthesis and properties of arylvinylidene-bridged triphenylamines.
;
_journal_issue                   4
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              2418
_journal_page_last               2424
_journal_paper_doi               10.1021/jo502605e
_journal_volume                  80
_journal_year                    2015
_chemical_formula_moiety         'C93 H93 N S3 Si3, 2(C4 H8 O2)'
_chemical_formula_sum            'C101 H109 N O4 S3 Si3'
_chemical_formula_weight         1581.34
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-06-28
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled 2012.03.27 svn.r2268, GUI svn.r4156)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.9240(4)
_cell_length_b                   37.2892(7)
_cell_length_c                   10.7444(2)
_cell_measurement_reflns_used    8234
_cell_measurement_temperature    173.00(10)
_cell_measurement_theta_max      61.5560
_cell_measurement_theta_min      4.7120
_cell_volume                     8783.9(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXH, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      173.00(10)
_diffrn_detector_area_resol_mean 10.6144
_diffrn_measured_fraction_theta_full 0.9903
_diffrn_measured_fraction_theta_max 0.9903
_diffrn_measurement_details
;
  1 omega  -56.00   30.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -      -43.5000   45.0000  -60.0000 86

  2 omega   64.00  109.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  -77.0000   90.0000 45

  3 omega   95.00  127.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  125.0000  -30.0000 32

  4 omega   45.00  110.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168 -125.0000  -30.0000 65

  5 omega  101.00  150.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  125.0000 -120.0000 49

  6 omega    9.00   36.00   1.0000   20.2800
omega____ theta____ kappa____ phi______ frames
    -       82.4168  -77.0000   90.0000 27
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0293449000
_diffrn_orient_matrix_UB_12      0.0375567000
_diffrn_orient_matrix_UB_13      -0.0008325000
_diffrn_orient_matrix_UB_21      -0.0084774000
_diffrn_orient_matrix_UB_22      0.0026030000
_diffrn_orient_matrix_UB_23      0.1420185000
_diffrn_orient_matrix_UB_31      0.0633113000
_diffrn_orient_matrix_UB_32      -0.0169966000
_diffrn_orient_matrix_UB_33      0.0196388000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0387
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            16074
_diffrn_reflns_theta_full        58.93
_diffrn_reflns_theta_max         58.93
_diffrn_reflns_theta_min         4.20
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.565
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69562
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour
;
;
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.196
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3376
_exptl_crystal_recrystallization_method 'crystallized from DCM/Hexane/EtOAc'
_exptl_crystal_size_max          0.2015
_exptl_crystal_size_mid          0.1145
_exptl_crystal_size_min          0.0494
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         6379
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.172
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0607
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0834P)²+9.8238P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1596
_refine_ls_wR_factor_ref         0.1680
_reflns_number_gt                5471
_reflns_number_total             6379
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo502605e_si_002.cif
_cod_data_source_block           nag12
_cod_depositor_comments
'Adding full bibliography for 4030570--4030572.cif.'
_cod_original_cell_volume        8783.8(3)
_cod_database_code               4030572
#BEGIN Tags that were not found in dictionaries:
_chemical_oxdiff_formula         'C87 H97 N S3 Si3'
_reflns_odcompleteness_completeness 99.03
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     58.86
#END Tags that were not found in dictionaries
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x+1/2, -y, z+1/2'
3 'x+1/2, -y+1/2, -z+1/2'
4 '-x, y+1/2, -z'
5 '-x, -y, -z'
6 'x-1/2, y, -z-1/2'
7 '-x-1/2, y-1/2, z-1/2'
8 'x, -y-1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C2 C 0.53847(13) 0.21778(8) -0.5753(3) 0.0247(7) Uani 1 1 d . . .
C3 C 0.48231(19) 0.2500 -0.4146(4) 0.0267(10) Uani 1 2 d S . .
C4 C 0.57110(19) 0.2500 -0.7638(4) 0.0270(10) Uani 1 2 d S . .
C5 C 0.57331(13) 0.21769(8) -0.6842(3) 0.0275(7) Uani 1 1 d . . .
C6 C 0.60989(14) 0.18824(8) -0.7108(3) 0.0299(7) Uani 1 1 d . . .
H6 H 0.6338 0.1883 -0.7823 0.036 Uiso 1 1 calc R . .
C7 C 0.61112(14) 0.15857(8) -0.6313(3) 0.0316(7) Uani 1 1 d . . .
C8 C 0.57007(14) 0.15730(8) -0.5324(3) 0.0315(7) Uani 1 1 d . . .
H8 H 0.5689 0.1371 -0.4817 0.038 Uiso 1 1 calc R . .
C9 C 0.53084(14) 0.18579(8) -0.5084(3) 0.0283(7) Uani 1 1 d . . .
C10 C 0.47752(14) 0.18344(8) -0.4240(3) 0.0273(7) Uani 1 1 d . . .
C11 C 0.46755(13) 0.21733(8) -0.3562(3) 0.0264(7) Uani 1 1 d . . .
C12 C 0.44388(14) 0.21795(9) -0.2361(3) 0.0297(7) Uani 1 1 d . . .
H12 H 0.4365 0.1964 -0.1951 0.036 Uiso 1 1 calc R . .
C13 C 0.43106(19) 0.2500 -0.1762(4) 0.0299(10) Uani 1 2 d S . .
C14 C 0.3990(2) 0.2500 -0.0595(4) 0.0340(11) Uani 1 2 d S . .
C15 C 0.3662(2) 0.2500 0.0306(5) 0.0448(13) Uani 1 2 d S . .
C16 C 0.3170(3) 0.20876(12) 0.2458(4) 0.0792(16) Uani 1 1 d D . .
H16A H 0.2973 0.1911 0.1915 0.095 Uiso 0.491(6) 1 calc PR A 2
H16 H 0.3250 0.1903 0.1830 0.095 Uiso 0.509(6) 1 calc PR A 1
C17 C 0.2773(4) 0.1922(3) 0.3262(9) 0.0592(13) Uani 0.509(6) 1 d PD A 1
H17A H 0.2610 0.2096 0.3831 0.089 Uiso 0.509(6) 1 calc PR A 1
H17B H 0.2985 0.1739 0.3720 0.089 Uiso 0.509(6) 1 calc PR A 1
H17C H 0.2446 0.1815 0.2797 0.089 Uiso 0.509(6) 1 calc PR A 1
C18 C 0.3853(4) 0.2142(2) 0.3149(9) 0.0592(13) Uani 0.509(6) 1 d PD A 1
H18A H 0.4141 0.2234 0.2554 0.089 Uiso 0.509(6) 1 calc PR A 1
H18B H 0.3994 0.1916 0.3461 0.089 Uiso 0.509(6) 1 calc PR A 1
H18C H 0.3815 0.2309 0.3826 0.089 Uiso 0.509(6) 1 calc PR A 1
C19 C 0.2319(2) 0.2500 0.0725(5) 0.0558(16) Uani 1 2 d SD . .
H19 H 0.2004 0.2500 0.1372 0.067 Uiso 1 2 calc SR A .
C20 C 0.2227(3) 0.21633(18) -0.0060(5) 0.100(2) Uani 1 1 d D A .
H20A H 0.1827 0.2167 -0.0422 0.149 Uiso 1 1 calc R . .
H20B H 0.2269 0.1955 0.0457 0.149 Uiso 1 1 calc R . .
H20C H 0.2527 0.2156 -0.0710 0.149 Uiso 1 1 calc R . .
C21 C 0.65173(15) 0.12942(9) -0.6574(3) 0.0351(8) Uani 1 1 d . . .
C22 C 0.68641(16) 0.10539(9) -0.6845(3) 0.0397(8) Uani 1 1 d . . .
C23 C 0.6904(2) 0.02824(13) -0.7476(6) 0.089(2) Uani 1 1 d D . .
H23 H 0.7169 0.0085 -0.7735 0.107 Uiso 1 1 calc R B 2
C24 C 0.7207(6) -0.0051(3) -0.7975(12) 0.077(3) Uani 0.428(9) 1 d PD C 1
H24A H 0.7400 -0.0178 -0.7305 0.115 Uiso 0.428(9) 1 calc PR C 1
H24B H 0.7507 0.0015 -0.8583 0.115 Uiso 0.428(9) 1 calc PR C 1
H24C H 0.6905 -0.0203 -0.8355 0.115 Uiso 0.428(9) 1 calc PR C 1
C24A C 0.6299(6) 0.0252(3) -0.6971(14) 0.077(3) Uani 0.428(9) 1 d PD C 1
H24D H 0.6030 0.0156 -0.7592 0.115 Uiso 0.428(9) 1 calc PR C 1
H24E H 0.6157 0.0485 -0.6723 0.115 Uiso 0.428(9) 1 calc PR C 1
H24F H 0.6305 0.0096 -0.6262 0.115 Uiso 0.428(9) 1 calc PR C 1
C26 C 0.8028(2) 0.06670(12) -0.6341(6) 0.0814(17) Uani 1 1 d D . .
H26 H 0.7826 0.0652 -0.5529 0.098 Uiso 0.673(8) 1 calc PR C 1
H26A H 0.8311 0.0518 -0.6822 0.098 Uiso 0.327(8) 1 calc PR C 2
C27 C 0.8428(4) 0.0347(2) -0.6329(9) 0.086(2) Uani 0.673(8) 1 d PD C 1
H27A H 0.8681 0.0347 -0.7058 0.128 Uiso 0.673(8) 1 calc PR C 1
H27B H 0.8181 0.0134 -0.6321 0.128 Uiso 0.673(8) 1 calc PR C 1
H27C H 0.8680 0.0352 -0.5599 0.128 Uiso 0.673(8) 1 calc PR C 1
C28 C 0.8383(2) 0.10150(14) -0.6238(5) 0.0786(15) Uani 1 1 d D C .
H28A H 0.8678 0.0995 -0.5582 0.118 Uiso 1 1 calc R . .
H28B H 0.8108 0.1208 -0.6058 0.118 Uiso 1 1 calc R . .
H28C H 0.8589 0.1062 -0.7011 0.118 Uiso 1 1 calc R . .
C29 C 0.7621(3) 0.08674(17) -0.9026(5) 0.0860(17) Uani 1 1 d . . .
H29 H 0.7936 0.1048 -0.8862 0.103 Uiso 1 1 calc R C .
C30 C 0.7121(4) 0.10597(19) -0.9772(5) 0.118(3) Uani 1 1 d . C .
H30A H 0.7298 0.1170 -1.0493 0.177 Uiso 1 1 calc R . .
H30B H 0.6934 0.1240 -0.9260 0.177 Uiso 1 1 calc R . .
H30C H 0.6819 0.0889 -1.0028 0.177 Uiso 1 1 calc R . .
C31 C 0.7921(3) 0.0585(2) -0.9817(7) 0.140(3) Uani 1 1 d . C .
H31A H 0.7631 0.0399 -1.0004 0.210 Uiso 1 1 calc R . .
H31B H 0.8260 0.0483 -0.9373 0.210 Uiso 1 1 calc R . .
H31C H 0.8063 0.0691 -1.0577 0.210 Uiso 1 1 calc R . .
C32 C 0.56524(19) 0.2500 -0.8892(4) 0.0276(10) Uani 1 2 d S . .
C33 C 0.56108(14) 0.21667(8) -0.9656(3) 0.0310(7) Uani 1 1 d . . .
C34 C 0.52072(15) 0.18897(8) -0.9381(3) 0.0356(8) Uani 1 1 d . . .
H34 H 0.4949 0.1909 -0.8697 0.043 Uiso 1 1 calc R . .
C35 C 0.51874(18) 0.15864(9) -1.0118(4) 0.0470(9) Uani 1 1 d . . .
H35 H 0.4919 0.1402 -0.9921 0.056 Uiso 1 1 calc R . .
C36 C 0.55607(19) 0.15540(10) -1.1141(4) 0.0525(10) Uani 1 1 d . . .
H36 H 0.5555 0.1345 -1.1611 0.063 Uiso 1 1 calc R . .
C37 C 0.59427(18) 0.18322(10) -1.1468(4) 0.0484(10) Uani 1 1 d . . .
H37 H 0.6186 0.1814 -1.2174 0.058 Uiso 1 1 calc R . .
C38 C 0.59634(15) 0.21413(9) -1.0737(3) 0.0362(8) Uani 1 1 d . . .
C39 C 0.43967(14) 0.15474(8) -0.4204(3) 0.0301(7) Uani 1 1 d . . .
C40 C 0.38146(15) 0.15418(8) -0.3492(3) 0.0309(7) Uani 1 1 d . . .
C41 C 0.33708(15) 0.18047(9) -0.3611(3) 0.0359(8) Uani 1 1 d . . .
H41 H 0.3436 0.1996 -0.4150 0.043 Uiso 1 1 calc R . .
C42 C 0.28343(16) 0.17864(11) -0.2942(4) 0.0457(9) Uani 1 1 d . . .
H42 H 0.2543 0.1966 -0.3027 0.055 Uiso 1 1 calc R . .
C43 C 0.27278(18) 0.15028(11) -0.2150(4) 0.0528(10) Uani 1 1 d . . .
H43 H 0.2372 0.1496 -0.1679 0.063 Uiso 1 1 calc R . .
C44 C 0.31448(18) 0.12312(11) -0.2057(4) 0.0496(10) Uani 1 1 d . . .
H44 H 0.3065 0.1036 -0.1542 0.060 Uiso 1 1 calc R . .
C45 C 0.36882(16) 0.12446(9) -0.2727(3) 0.0379(8) Uani 1 1 d . . .
C46 C 0.44528(16) 0.08823(9) -0.4205(3) 0.0402(8) Uani 1 1 d . . .
C47 C 0.45775(18) 0.05539(10) -0.4761(4) 0.0527(10) Uani 1 1 d . . .
H47 H 0.4557 0.0344 -0.4295 0.063 Uiso 1 1 calc R . .
C48 C 0.47311(19) 0.05392(11) -0.5996(4) 0.0580(11) Uani 1 1 d . . .
H48 H 0.4824 0.0320 -0.6366 0.070 Uiso 1 1 calc R . .
C49 C 0.47477(18) 0.08521(11) -0.6690(4) 0.0512(10) Uani 1 1 d . . .
H49 H 0.4839 0.0842 -0.7535 0.061 Uiso 1 1 calc R . .
C50 C 0.46295(15) 0.11775(10) -0.6139(3) 0.0399(8) Uani 1 1 d . . .
H50 H 0.4633 0.1385 -0.6621 0.048 Uiso 1 1 calc R . .
C51 C 0.45042(14) 0.12016(9) -0.4869(3) 0.0342(8) Uani 1 1 d . . .
N1 N 0.51026(15) 0.2500 -0.5343(3) 0.0255(8) Uani 1 2 d S . .
Si1 Si 0.30729(6) 0.2500 0.15233(12) 0.0325(3) Uani 1 2 d S . .
Si2 Si 0.73595(5) 0.07024(3) -0.74507(10) 0.0459(3) Uani 1 1 d . C .
S1 S 0.64364(6) 0.2500 -1.11940(13) 0.0485(4) Uani 1 2 d S . .
S2 S 0.42153(5) 0.08907(2) -0.26255(9) 0.0504(3) Uani 1 1 d . . .
C27A C 0.7929(7) 0.0458(4) -0.5333(15) 0.086(2) Uani 0.327(8) 1 d PD C 2
H27D H 0.7773 0.0229 -0.5596 0.128 Uiso 0.327(8) 1 calc PR C 2
H27E H 0.7639 0.0572 -0.4794 0.128 Uiso 0.327(8) 1 calc PR C 2
H27F H 0.8306 0.0423 -0.4893 0.128 Uiso 0.327(8) 1 calc PR C 2
C25A C 0.6386(4) 0.0293(3) -0.8286(10) 0.085(3) Uani 0.572(9) 1 d PD C 2
H25A H 0.6520 0.0337 -0.9124 0.127 Uiso 0.572(9) 1 calc PR C 2
H25B H 0.6117 0.0482 -0.8029 0.127 Uiso 0.572(9) 1 calc PR C 2
H25C H 0.6175 0.0068 -0.8251 0.127 Uiso 0.572(9) 1 calc PR C 2
C1B C 0.6572(3) 0.07930(18) -0.3257(6) 0.0961(18) Uani 1 1 d . . .
H1BA H 0.6727 0.0757 -0.4083 0.144 Uiso 1 1 calc R . .
H1BB H 0.6894 0.0758 -0.2664 0.144 Uiso 1 1 calc R . .
H1BC H 0.6416 0.1033 -0.3182 0.144 Uiso 1 1 calc R . .
O2 O 0.51755(17) 0.01726(9) -0.2002(3) 0.0793(10) Uani 1 1 d . . .
O1 O 0.58528(15) 0.06048(8) -0.1776(3) 0.0688(9) Uani 1 1 d . . .
C1C C 0.6081(2) 0.05363(15) -0.3017(5) 0.0760(14) Uani 1 1 d . . .
H1CA H 0.5757 0.0566 -0.3623 0.091 Uiso 1 1 calc R . .
H1CB H 0.6235 0.0293 -0.3076 0.091 Uiso 1 1 calc R . .
C1A C 0.5185(3) 0.05095(14) -0.0117(4) 0.0769(14) Uani 1 1 d . . .
H1AA H 0.5239 0.0314 0.0453 0.115 Uiso 1 1 calc R . .
H1AB H 0.4760 0.0571 -0.0162 0.115 Uiso 1 1 calc R . .
H1AC H 0.5413 0.0713 0.0168 0.115 Uiso 1 1 calc R . .
C1 C 0.5405(2) 0.04018(11) -0.1377(4) 0.0561(11) Uani 1 1 d . . .
C25 C 0.6655(5) 0.0200(3) -0.6164(9) 0.085(3) Uani 0.572(9) 1 d PD C 2
H25D H 0.6481 -0.0036 -0.6154 0.127 Uiso 0.572(9) 1 calc PR C 2
H25E H 0.6347 0.0372 -0.5950 0.127 Uiso 0.572(9) 1 calc PR C 2
H25F H 0.6982 0.0212 -0.5570 0.127 Uiso 0.572(9) 1 calc PR C 2
C17A C 0.2641(4) 0.2125(3) 0.3600(9) 0.0592(13) Uani 0.491(6) 1 d PD A 2
H17D H 0.2775 0.2298 0.4203 0.089 Uiso 0.491(6) 1 calc PR A 2
H17E H 0.2586 0.1897 0.3997 0.089 Uiso 0.491(6) 1 calc PR A 2
H17F H 0.2260 0.2202 0.3246 0.089 Uiso 0.491(6) 1 calc PR A 2
C18A C 0.3660(4) 0.1902(2) 0.2830(9) 0.0592(13) Uani 0.491(6) 1 d PD A 2
H18D H 0.3888 0.1825 0.2115 0.089 Uiso 0.491(6) 1 calc PR A 2
H18E H 0.3531 0.1696 0.3298 0.089 Uiso 0.491(6) 1 calc PR A 2
H18F H 0.3912 0.2051 0.3343 0.089 Uiso 0.491(6) 1 calc PR A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
13 -10 1 0.0492 12.7671 -9.9705 1.1168 -0.0007 0.0244 0.9997
8 -4 -6 0.0931 7.9383 -4.4516 -5.6500 0.0705 -0.8813 0.4673
-3 4 -7 0.0837 -3.1094 4.1984 -6.6969 0.0720 -0.9138 -0.3997
-13 9 1 0.0378 -12.8717 9.3985 1.2466 -0.0258 0.3106 -0.9502
14 5 1 0.0410 13.6838 5.4344 1.0645 0.6048 0.0493 0.7949
1 24 0 0.0155 1.2986 24.0988 0.1587 0.9430 0.0743 -0.3243
-14 3 -1 0.0633 -13.9411 3.0931 -1.0634 -0.2920 -0.0248 -0.9561
1 -24 0 0.0257 0.6931 -24.1825 -0.0059 -0.8879 -0.0697 0.4548
2 -4 7 0.0959 1.9783 -3.9893 7.0050 -0.0976 0.9677 0.3306
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
C5 C2 C9 119.5(3) . .
C5 C2 N1 120.0(3) . .
C9 C2 N1 120.5(3) . .
C11 C3 C11 119.8(4) . 8_565
C11 C3 N1 120.07(19) 8_565 .
C11 C3 N1 120.07(19) . .
C5 C4 C5 109.2(4) 8_565 .
C32 C4 C5 125.38(18) . .
C32 C4 C5 125.38(18) . 8_565
C2 C5 C4 117.7(3) . .
C6 C5 C2 119.3(3) . .
C6 C5 C4 122.9(3) . .
C5 C6 C7 120.7(3) . .
C6 C7 C21 119.5(3) . .
C8 C7 C6 118.7(3) . .
C8 C7 C21 121.7(3) . .
C9 C8 C7 121.0(3) . .
C2 C9 C10 117.3(3) . .
C8 C9 C2 118.7(3) . .
C8 C9 C10 123.8(3) . .
C11 C10 C9 111.6(3) . .
C39 C10 C9 123.2(3) . .
C39 C10 C11 124.9(3) . .
C3 C11 C10 119.2(3) . .
C12 C11 C3 119.0(3) . .
C12 C11 C10 121.8(3) . .
C13 C12 C11 121.3(3) . .
C12 C13 C12 119.2(4) 8_565 .
C12 C13 C14 120.3(2) . .
C12 C13 C14 120.3(2) 8_565 .
C15 C14 C13 172.7(5) . .
C14 C15 Si1 171.9(5) . .
C17 C16 C18 110.0(6) . .
C17 C16 Si1 130.0(5) . .
C17 C16 C17A 31.5(5) . .
C18 C16 Si1 104.0(4) . .
C18 C16 C17A 106.3(6) . .
C17A C16 Si1 104.2(4) . .
C18A C16 C17 95.1(6) . .
C18A C16 C18 38.5(5) . .
C18A C16 Si1 133.2(5) . .
C18A C16 C17A 112.1(6) . .
C20 C19 C20 110.7(6) 8_565 .
C20 C19 Si1 111.9(3) . .
C20 C19 Si1 111.9(3) 8_565 .
C22 C21 C7 177.2(4) . .
C21 C22 Si2 173.0(3) . .
C24 C23 Si2 117.6(5) . .
C24 C23 C25 108.4(7) . .
C24A C23 C24 118.4(7) . .
C24A C23 Si2 123.8(5) . .
C24A C23 C25 46.6(6) . .
C25A C23 C24 99.0(8) . .
C25A C23 C24A 60.0(7) . .
C25A C23 Si2 114.3(5) . .
C25A C23 C25 106.3(7) . .
C25 C23 Si2 110.2(5) . .
C27 C26 C28 112.7(5) . .
C27 C26 Si2 121.3(5) . .
C28 C26 Si2 112.5(4) . .
C27A C26 C27 67.8(8) . .
C27A C26 C28 121.2(9) . .
C27A C26 Si2 114.8(8) . .
C30 C29 Si2 113.7(4) . .
C31 C29 C30 110.2(5) . .
C31 C29 Si2 114.2(5) . .
C4 C32 C33 123.59(18) . 8_565
C4 C32 C33 123.59(18) . .
C33 C32 C33 112.8(4) . 8_565
C34 C33 C32 122.7(3) . .
C34 C33 C38 118.5(3) . .
C38 C33 C32 118.6(3) . .
C35 C34 C33 120.4(3) . .
C36 C35 C34 120.7(4) . .
C35 C36 C37 119.9(3) . .
C36 C37 C38 119.9(4) . .
C33 C38 S1 120.4(3) . .
C37 C38 C33 120.3(3) . .
C37 C38 S1 119.3(3) . .
C10 C39 C40 123.4(3) . .
C10 C39 C51 124.9(3) . .
C40 C39 C51 111.7(3) . .
C41 C40 C39 122.9(3) . .
C41 C40 C45 118.2(3) . .
C45 C40 C39 118.7(3) . .
C42 C41 C40 121.0(3) . .
C43 C42 C41 120.3(4) . .
C44 C43 C42 120.0(3) . .
C43 C44 C45 120.5(4) . .
C40 C45 S2 119.9(3) . .
C44 C45 C40 119.9(3) . .
C44 C45 S2 120.2(3) . .
C47 C46 C51 121.1(4) . .
C47 C46 S2 119.0(3) . .
C51 C46 S2 119.9(3) . .
C48 C47 C46 120.0(4) . .
C47 C48 C49 119.6(4) . .
C50 C49 C48 120.4(4) . .
C49 C50 C51 121.0(4) . .
C46 C51 C39 118.7(3) . .
C46 C51 C50 117.5(3) . .
C50 C51 C39 123.7(3) . .
C2 N1 C2 115.4(3) 8_565 .
C2 N1 C3 117.85(19) . .
C2 N1 C3 117.86(19) 8_565 .
C15 Si1 C16 107.77(19) . .
C15 Si1 C16 107.77(19) . 8_565
C15 Si1 C19 107.2(2) . .
C16 Si1 C16 112.5(3) 8_565 .
C16 Si1 C19 110.7(2) . .
C16 Si1 C19 110.7(2) 8_565 .
C22 Si2 C23 106.92(19) . .
C22 Si2 C26 106.6(2) . .
C22 Si2 C29 105.5(2) . .
C23 Si2 C26 111.5(3) . .
C23 Si2 C29 115.1(3) . .
C29 Si2 C26 110.6(3) . .
C38 S1 C38 98.8(2) . 8_565
C45 S2 C46 98.43(16) . .
C1 O1 C1C 117.3(3) . .
O1 C1C C1B 107.5(4) . .
O2 C1 O1 122.9(4) . .
O2 C1 C1A 124.3(4) . .
O1 C1 C1A 112.5(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C2 C5 1.397(4) .
C2 C9 1.403(4) .
C2 N1 1.421(3) .
C3 C11 1.408(4) 8_565
C3 C11 1.408(4) .
C3 N1 1.425(5) .
C4 C5 1.479(4) .
C4 C5 1.479(4) 8_565
C4 C32 1.354(6) .
C5 C6 1.389(4) .
C6 C7 1.398(4) .
C7 C8 1.393(4) .
C7 C21 1.433(5) .
C8 C9 1.391(4) .
C9 C10 1.482(4) .
C10 C11 1.475(4) .
C10 C39 1.355(4) .
C11 C12 1.391(4) .
C12 C13 1.386(4) .
C13 C12 1.386(4) 8_565
C13 C14 1.437(6) .
C14 C15 1.207(7) .
C15 Si1 1.838(5) .
C16 C17 1.374(9) .
C16 C18 1.684(9) .
C16 Si1 1.849(5) .
C16 C17A 1.695(9) .
C16 C18A 1.338(9) .
C19 C20 1.526(6) 8_565
C19 C20 1.526(6) .
C19 Si1 1.861(5) .
C21 C22 1.211(5) .
C22 Si2 1.823(4) .
C23 C24 1.509(10) .
C23 C24A 1.437(11) .
C23 Si2 1.857(5) .
C23 C25A 1.431(10) .
C23 C25 1.543(10) .
C26 C27 1.481(7) .
C26 C28 1.517(6) .
C26 Si2 1.894(5) .
C26 C27A 1.352(14) .
C29 C30 1.535(9) .
C29 C31 1.505(8) .
C29 Si2 1.891(5) .
C32 C33 1.492(4) 8_565
C32 C33 1.492(4) .
C33 C34 1.392(5) .
C33 C38 1.398(5) .
C34 C35 1.382(5) .
C35 C36 1.375(6) .
C36 C37 1.379(6) .
C37 C38 1.395(5) .
C38 S1 1.762(3) .
C39 C40 1.488(4) .
C39 C51 1.493(4) .
C40 C41 1.387(5) .
C40 C45 1.407(5) .
C41 C42 1.380(5) .
C42 C43 1.378(6) .
C43 C44 1.368(6) .
C44 C45 1.393(5) .
C45 S2 1.758(4) .
C46 C47 1.390(5) .
C46 C51 1.393(5) .
C46 S2 1.775(4) .
C47 C48 1.369(6) .
C48 C49 1.386(6) .
C49 C50 1.375(5) .
C50 C51 1.395(5) .
N1 C2 1.421(3) 8_565
Si1 C16 1.849(5) 8_565
S1 C38 1.762(3) 8_565
C1B C1C 1.462(7) .
O2 C1 1.198(5) .
O1 C1C 1.447(6) .
O1 C1 1.311(5) .
C1A C1 1.493(6) .
