#------------------------------------------------------------------------------
#$Date: 2020-12-04 04:19:49 +0200 (Fri, 04 Dec 2020) $
#$Revision: 259516 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/53/4135339.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_4135339
loop_
_publ_author_name
'Bergman, Harrison M.'
'Kiel, Gavin R.'
'Witzke, Ryan J.'
'Nenon, David P.'
'Schwartzberg, Adam M.'
'Liu, Yi'
'Tilley, T. Don'
_publ_section_title
;
 Shape-Selective Synthesis of Pentacene Macrocycles and the Effect of
 Geometry on Singlet Fission.
;
_journal_issue                   47
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              19850
_journal_page_last               19855
_journal_paper_doi               10.1021/jacs.0c09941
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C108 H112 Si4, 2(C4 H8 O)'
_chemical_formula_sum            'C108 H112 O Si4'
_chemical_formula_weight         1538.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.212(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.5851(11)
_cell_length_b                   14.7231(8)
_cell_length_c                   15.1871(8)
_cell_measurement_reflns_used    9773
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.48
_cell_measurement_theta_min      2.40
_cell_volume                     4813.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 7.39
_diffrn_detector_type            'Bruker-Nonius APEXII CCD area detector'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker D8 with PHOTON 100 detector'
_diffrn_measurement_device_type  'Bruker D8 diffractometer'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0765
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            52169
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        24.535
_diffrn_reflns_theta_max         24.535
_diffrn_reflns_theta_min         1.718
_diffrn_source                   'Bend magnet, Station 12.2.1, ALS, LBNL'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.7451
_exptl_absorpt_correction_T_min  0.6416
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1729 before and 0.0829 after correction. The Ratio of minimum to maximum transmission is 0.8611. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       needle
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.852
_refine_diff_density_min         -0.742
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     582
_refine_ls_number_reflns         7402
_refine_ls_number_restraints     97
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0899
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1325P)²+10.5103P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2502
_refine_ls_wR_factor_ref         0.2642
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5991
_reflns_number_total             7402
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja0c09941_si_004.cif
_cod_data_source_block           hb1f
_cod_depositor_comments
'Adding full bibliography for 4135339--4135341.cif.'
_cod_database_code               4135339
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.997
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C51, C53, C55, C52, C57, C54, C56
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
3. Uiso/Uaniso restraints and constraints
C51 \\sim C53 \\sim C55 \\sim C52 \\sim C57 \\sim C54 \\sim C56: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C44, C45, C46, C47
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Fixed Sof: H51A(0.5) H51B(0.5) H51C(0.5) H51D(0.5) C53(0.5) H53A(0.5)
 H53B(0.5) C55(0.5) H55A(0.5) H55B(0.5) C52(0.5) H52A(0.5) H52B(0.5) C57(0.5)
 H57A(0.5) H57B(0.5) H57C(0.5) C54(0.5) H54A(0.5) H54B(0.5) H54C(0.5) C56(0.5)
 H56A(0.5) H56B(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C60(H60A,H60B), C61(H61A,H61B), C58(H58A,H58B), C59(H59A,H59B), C44(H44A,
 H44B), C45(H45A,H45B), C46(H46A,H46B), C51(H51A,H51B), C51(H51C,H51D),
 C53(H53A,H53B), C55(H55A,H55B), C52(H52A,H52B), C56(H56A,H56B)
6.b Me refined with riding coordinates:
 C57(H57A,H57B,H57C), C54(H54A,H54B,H54C)
6.c Aromatic/amide H refined with riding coordinates:
 C19(H19), C13(H13), C20(H20), C3(H3), C10(H10), C26(H26), C37(H37), C12(H12),
 C34(H34), C40(H40), C25(H25), C33(H33), C39(H39), C31(H31), C30(H30), C36(H36),
  C6(H6), C23(H23), C11(H11), C22(H22), C17(H17), C16(H16), C5(H5), C48(H48),
 C4(H4), C41(H41)
6.d Idealised Me refined as rotating group:
 C49(H49A,H49B,H49C), C43(H43A,H43B,H43C), C50(H50A,H50B,H50C), C47(H47A,H47B,
 H47C), C42(H42A,H42B,H42C)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Si2 Si 0.85721(6) 0.17968(9) -0.07410(9) 0.0435(4) Uani 1 1 d . . . . .
Si1 Si 0.90914(7) 0.62152(9) -0.08520(10) 0.0510(4) Uani 1 1 d . . . . .
C14 C 0.45736(17) 0.2418(3) 0.4187(2) 0.0259(8) Uani 1 1 d . . . . .
C9 C 0.41547(18) 0.2522(3) 0.4875(2) 0.0268(8) Uani 1 1 d . . . . .
C15 C 0.52391(18) 0.3091(3) 0.3071(2) 0.0279(9) Uani 1 1 d . . . . .
C1 C 0.47711(18) 0.3191(3) 0.3743(2) 0.0270(9) Uani 1 1 d . . . . .
C19 C 0.55418(19) 0.3188(3) 0.1561(2) 0.0287(9) Uani 1 1 d . . . . .
H19 H 0.5428 0.3282 0.0952 0.034 Uiso 1 1 calc R . . . .
C8 C 0.39472(18) 0.3384(3) 0.5104(2) 0.0276(9) Uani 1 1 d . . . . .
C18 C 0.61559(19) 0.3005(3) 0.1836(3) 0.0297(9) Uani 1 1 d . . . . .
C7 C 0.41347(18) 0.4163(3) 0.4648(2) 0.0298(9) Uani 1 1 d . . . . .
C21 C 0.66653(19) 0.3055(3) 0.1230(3) 0.0307(9) Uani 1 1 d . . . . .
C13 C 0.47630(18) 0.1524(3) 0.3969(2) 0.0282(9) Uani 1 1 d . . . . .
H13 H 0.5040 0.1446 0.3517 0.034 Uiso 1 1 calc R . . . .
C35 C 0.72147(19) 0.6184(3) 0.2739(2) 0.0302(9) Uani 1 1 d . . . . .
C2 C 0.45524(18) 0.4058(3) 0.3954(2) 0.0293(9) Uani 1 1 d . . . . .
C20 C 0.50887(19) 0.3237(3) 0.2169(2) 0.0279(9) Uani 1 1 d . . . . .
H20 H 0.4671 0.3370 0.1969 0.034 Uiso 1 1 calc R . . . .
C3 C 0.47389(19) 0.4862(3) 0.3514(3) 0.0340(9) Uani 1 1 d . . . . .
H3 H 0.5025 0.4813 0.3070 0.041 Uiso 1 1 calc R . . . .
C38 C 0.64684(19) 0.6502(3) 0.4149(2) 0.0294(9) Uani 1 1 d . . . . .
C29 C 0.81763(19) 0.5167(3) 0.0562(3) 0.0322(9) Uani 1 1 d . . . . .
C27 C 0.82685(19) 0.3659(3) -0.0208(3) 0.0331(9) Uani 1 1 d . . . . .
C32 C 0.75889(19) 0.5914(3) 0.1994(2) 0.0304(9) Uani 1 1 d . . . . .
C10 C 0.39540(18) 0.1718(3) 0.5303(2) 0.0290(9) Uani 1 1 d . . . . .
H10 H 0.3677 0.1775 0.5758 0.035 Uiso 1 1 calc R . . . .
C26 C 0.66170(19) 0.3645(3) 0.0504(3) 0.0323(9) Uani 1 1 d . . . . .
H26 H 0.6232 0.3935 0.0346 0.039 Uiso 1 1 calc R . . . .
C37 C 0.62089(19) 0.6468(3) 0.3286(3) 0.0328(9) Uani 1 1 d . . . . .
H37 H 0.5774 0.6554 0.3170 0.039 Uiso 1 1 calc R . . . .
C12 C 0.45582(19) 0.0782(3) 0.4391(3) 0.0321(9) Uani 1 1 d . . . . .
H12 H 0.4689 0.0193 0.4227 0.038 Uiso 1 1 calc R . . . .
C28 C 0.84168(19) 0.4658(3) -0.0194(3) 0.0345(10) Uani 1 1 d . . . . .
C34 C 0.83408(19) 0.4895(3) 0.1424(3) 0.0343(10) Uani 1 1 d . . . . .
H34 H 0.8653 0.4446 0.1531 0.041 Uiso 1 1 calc R . . . .
C40 C 0.74741(19) 0.6250(3) 0.3605(3) 0.0339(9) Uani 1 1 d . . . . .
H40 H 0.7910 0.6185 0.3722 0.041 Uiso 1 1 calc R . . . .
C25 C 0.7123(2) 0.3813(3) 0.0012(3) 0.0357(10) Uani 1 1 d . . . . .
H25 H 0.7080 0.4219 -0.0474 0.043 Uiso 1 1 calc R . . . .
C24 C 0.7696(2) 0.3391(3) 0.0226(3) 0.0328(9) Uani 1 1 d . . . . .
C33 C 0.80597(19) 0.5263(3) 0.2125(3) 0.0328(9) Uani 1 1 d . . . . .
H33 H 0.8187 0.5072 0.2708 0.039 Uiso 1 1 calc R . . . .
C39 C 0.71045(19) 0.6409(3) 0.4294(3) 0.0340(9) Uani 1 1 d . . . . .
H39 H 0.7291 0.6455 0.4879 0.041 Uiso 1 1 calc R . . . .
C31 C 0.7449(2) 0.6226(3) 0.1134(3) 0.0342(9) Uani 1 1 d . . . . .
H31 H 0.7153 0.6699 0.1029 0.041 Uiso 1 1 calc R . . . .
C30 C 0.7737(2) 0.5853(3) 0.0432(3) 0.0344(10) Uani 1 1 d . . . . .
H30 H 0.7633 0.6070 -0.0148 0.041 Uiso 1 1 calc R . . . .
C36 C 0.65804(19) 0.6308(3) 0.2587(3) 0.0337(9) Uani 1 1 d . . . . .
H36 H 0.6395 0.6285 0.2000 0.040 Uiso 1 1 calc R . . . .
C6 C 0.39276(19) 0.5052(3) 0.4851(3) 0.0339(10) Uani 1 1 d . . . . .
H6 H 0.3660 0.5130 0.5315 0.041 Uiso 1 1 calc R . . . .
C23 C 0.7731(2) 0.2771(3) 0.0916(3) 0.0360(10) Uani 1 1 d . . . . .
H23 H 0.8110 0.2456 0.1054 0.043 Uiso 1 1 calc R . . . .
C11 C 0.4148(2) 0.0881(3) 0.5079(3) 0.0338(9) Uani 1 1 d . . . . .
H11 H 0.4011 0.0361 0.5379 0.041 Uiso 1 1 calc R . . . .
C22 C 0.72287(19) 0.2599(3) 0.1408(3) 0.0346(10) Uani 1 1 d . . . . .
H22 H 0.7267 0.2165 0.1872 0.041 Uiso 1 1 calc R . . . .
C17 C 0.6296(2) 0.2814(3) 0.2733(3) 0.0360(10) Uani 1 1 d . . . . .
H17 H 0.6708 0.2650 0.2931 0.043 Uiso 1 1 calc R . . . .
C16 C 0.58461(19) 0.2859(3) 0.3335(3) 0.0354(10) Uani 1 1 d . . . . .
H16 H 0.5956 0.2729 0.3939 0.042 Uiso 1 1 calc R . . . .
C5 C 0.4103(2) 0.5792(3) 0.4396(3) 0.0392(10) Uani 1 1 d . . . . .
H5 H 0.3950 0.6376 0.4533 0.047 Uiso 1 1 calc R . . . .
C48 C 0.8649(2) 0.3046(3) -0.0538(3) 0.0368(10) Uani 1 1 d . . . . .
H48 H 0.9030 0.3294 -0.0699 0.044 Uiso 1 1 calc R . . . .
C4 C 0.4516(2) 0.5694(3) 0.3718(3) 0.0394(10) Uani 1 1 d . . . . .
H4 H 0.4639 0.6213 0.3403 0.047 Uiso 1 1 calc R . . . .
C41 C 0.8746(2) 0.5056(3) -0.0806(3) 0.0402(11) Uani 1 1 d . . . . .
H41 H 0.8813 0.4684 -0.1300 0.048 Uiso 1 1 calc R . . . .
O1 O 0.6952(3) 0.5420(3) -0.1755(3) 0.0993(17) Uani 1 1 d . . . . .
C49 C 0.7751(2) 0.1413(4) -0.0977(4) 0.0626(15) Uani 1 1 d . . . . .
H49A H 0.7476 0.1785 -0.0639 0.094 Uiso 1 1 calc GR . . . .
H49B H 0.7714 0.0775 -0.0806 0.094 Uiso 1 1 calc GR . . . .
H49C H 0.7633 0.1479 -0.1609 0.094 Uiso 1 1 calc GR . . . .
C60 C 0.7222(3) 0.6088(5) -0.3070(4) 0.0698(17) Uani 1 1 d . . . . .
H60A H 0.7565 0.6532 -0.3091 0.084 Uiso 1 1 calc R . . . .
H60B H 0.6934 0.6161 -0.3603 0.084 Uiso 1 1 calc R . . . .
C43 C 0.9862(3) 0.6079(4) -0.1308(5) 0.0708(18) Uani 1 1 d . . . . .
H43A H 1.0127 0.5691 -0.0915 0.106 Uiso 1 1 calc GR . . . .
H43B H 1.0057 0.6676 -0.1357 0.106 Uiso 1 1 calc GR . . . .
H43C H 0.9807 0.5799 -0.1894 0.106 Uiso 1 1 calc GR . . . .
C61 C 0.6897(3) 0.6199(5) -0.2265(4) 0.0711(17) Uani 1 1 d . . . . .
H61A H 0.7075 0.6721 -0.1922 0.085 Uiso 1 1 calc R . . . .
H61B H 0.6453 0.6327 -0.2423 0.085 Uiso 1 1 calc R . . . .
C50 C 0.9008(3) 0.1596(5) -0.1733(5) 0.091(3) Uani 1 1 d . . . . .
H50A H 0.8773 0.1846 -0.2255 0.137 Uiso 1 1 calc GR . . . .
H50B H 0.9067 0.0942 -0.1812 0.137 Uiso 1 1 calc GR . . . .
H50C H 0.9414 0.1895 -0.1656 0.137 Uiso 1 1 calc GR . . . .
C58 C 0.7090(4) 0.4690(5) -0.2340(4) 0.0798(19) Uani 1 1 d . . . . .
H58A H 0.6703 0.4440 -0.2634 0.096 Uiso 1 1 calc R . . . .
H58B H 0.7313 0.4195 -0.2008 0.096 Uiso 1 1 calc R . . . .
C47 C 0.9875(4) 0.6232(6) 0.2650(6) 0.106(2) Uani 1 1 d . U . . .
H47A H 1.0321 0.6260 0.2567 0.160 Uiso 1 1 calc GR . . . .
H47B H 0.9739 0.5597 0.2634 0.160 Uiso 1 1 calc GR . . . .
H47C H 0.9796 0.6499 0.3222 0.160 Uiso 1 1 calc GR . . . .
C42 C 0.8588(3) 0.6942(5) -0.1583(6) 0.098(3) Uani 1 1 d . . . . .
H42A H 0.8486 0.6627 -0.2143 0.147 Uiso 1 1 calc GR . . . .
H42B H 0.8804 0.7511 -0.1694 0.147 Uiso 1 1 calc GR . . . .
H42C H 0.8204 0.7076 -0.1300 0.147 Uiso 1 1 calc GR . . . .
C59 C 0.7483(4) 0.5080(6) -0.2994(5) 0.093(2) Uani 1 1 d . . . . .
H59A H 0.7427 0.4757 -0.3566 0.112 Uiso 1 1 calc R . . . .
H59B H 0.7927 0.5070 -0.2781 0.112 Uiso 1 1 calc R . . . .
C44 C 0.9176(4) 0.6809(6) 0.0234(6) 0.103(2) Uani 1 1 d . U . . .
H44A H 0.9362 0.7413 0.0140 0.123 Uiso 1 1 calc R . . . .
H44B H 0.8755 0.6913 0.0432 0.123 Uiso 1 1 calc R . . . .
C45 C 0.9533(5) 0.6377(7) 0.0925(7) 0.123(3) Uani 1 1 d . U . . .
H45A H 0.9973 0.6384 0.0780 0.148 Uiso 1 1 calc R . . . .
H45B H 0.9402 0.5733 0.0943 0.148 Uiso 1 1 calc R . . . .
C46 C 0.9497(6) 0.6791(8) 0.1871(7) 0.149(4) Uani 1 1 d . U . . .
H46A H 0.9055 0.6823 0.2003 0.178 Uiso 1 1 calc R . . . .
H46B H 0.9659 0.7419 0.1869 0.178 Uiso 1 1 calc R . . . .
C51 C 0.8920(4) 0.1138(5) 0.0195(6) 0.096(2) Uani 1 1 d . U . . .
H51A H 0.9375 0.1236 0.0217 0.115 Uiso 0.5 1 calc R . P A 1
H51B H 0.8774 0.1407 0.0739 0.115 Uiso 0.5 1 calc R . P A 1
H51C H 0.9300 0.1437 0.0462 0.115 Uiso 0.5 1 calc R . P B 2
H51D H 0.8623 0.1053 0.0653 0.115 Uiso 0.5 1 calc R . P B 2
C53 C 0.9408(9) -0.0461(12) 0.0475(14) 0.115(3) Uani 0.5 1 d . U P C 2
H53A H 0.9501 -0.0042 0.0977 0.139 Uiso 0.5 1 calc R . P C 2
H53B H 0.9816 -0.0622 0.0258 0.139 Uiso 0.5 1 calc R . P C 2
C55 C 0.8815(10) 0.0139(13) 0.0238(14) 0.114(3) Uani 0.5 1 d . U P D 1
H55A H 0.9012 -0.0135 -0.0266 0.137 Uiso 0.5 1 calc R . P D 1
H55B H 0.8362 0.0040 0.0130 0.137 Uiso 0.5 1 calc R . P D 1
C52 C 0.9089(9) 0.0151(12) -0.0270(13) 0.109(3) Uani 0.5 1 d . U P C 2
H52A H 0.8706 -0.0143 -0.0530 0.131 Uiso 0.5 1 calc R . P C 2
H52B H 0.9373 0.0249 -0.0744 0.131 Uiso 0.5 1 calc R . P C 2
C57 C 0.9169(12) -0.1401(17) 0.0929(17) 0.153(5) Uani 0.5 1 d . U P C 2
H57A H 0.9485 -0.1610 0.1380 0.229 Uiso 0.5 1 calc R . P C 2
H57B H 0.8780 -0.1282 0.1204 0.229 Uiso 0.5 1 calc R . P C 2
H57C H 0.9099 -0.1870 0.0475 0.229 Uiso 0.5 1 calc R . P C 2
C54 C 0.8643(11) -0.1166(17) 0.0666(17) 0.149(5) Uani 0.5 1 d . U P D 1
H54A H 0.8626 -0.1743 0.0985 0.224 Uiso 0.5 1 calc R . P D 1
H54B H 0.8225 -0.0908 0.0580 0.224 Uiso 0.5 1 calc R . P D 1
H54C H 0.8807 -0.1272 0.0090 0.224 Uiso 0.5 1 calc R . P D 1
C56 C 0.9065(9) -0.0508(12) 0.1197(13) 0.110(3) Uani 0.5 1 d . U P D 1
H56A H 0.9511 -0.0670 0.1254 0.132 Uiso 0.5 1 calc R . P D 1
H56B H 0.8911 -0.0295 0.1759 0.132 Uiso 0.5 1 calc R . P D 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017 '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'
O O 0.0115 0.0064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0864 0.0750 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C49 Si2 C48 113.6(2) . . ?
C50 Si2 C48 104.3(3) . . ?
C50 Si2 C49 109.0(3) . . ?
C51 Si2 C48 111.5(3) . . ?
C51 Si2 C49 108.5(3) . . ?
C51 Si2 C50 109.9(4) . . ?
C43 Si1 C41 106.7(2) . . ?
C43 Si1 C44 110.4(3) . . ?
C42 Si1 C41 109.5(3) . . ?
C42 Si1 C43 110.1(3) . . ?
C42 Si1 C44 106.0(4) . . ?
C44 Si1 C41 114.2(3) . . ?
C1 C14 C9 119.4(3) . . ?
C1 C14 C13 122.3(3) . . ?
C13 C14 C9 118.3(3) . . ?
C8 C9 C14 120.5(3) . . ?
C8 C9 C10 121.6(3) . . ?
C10 C9 C14 117.9(3) . . ?
C20 C15 C1 122.2(3) . . ?
C16 C15 C1 120.0(3) . . ?
C16 C15 C20 117.8(3) . . ?
C14 C1 C15 119.5(3) . . ?
C14 C1 C2 120.5(3) . . ?
C2 C1 C15 120.0(3) . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.8(4) . . ?
C20 C19 H19 119.6 . . ?
C9 C8 C7 120.4(3) . . ?
C9 C8 C38 120.5(3) . 3_666 ?
C7 C8 C38 119.1(3) . 3_666 ?
C19 C18 C21 122.5(4) . . ?
C19 C18 C17 117.7(4) . . ?
C17 C18 C21 119.7(4) . . ?
C8 C7 C2 119.1(3) . . ?
C8 C7 C6 122.3(3) . . ?
C6 C7 C2 118.6(4) . . ?
C26 C21 C18 120.1(4) . . ?
C22 C21 C18 121.9(4) . . ?
C22 C21 C26 117.6(4) . . ?
C14 C13 H13 119.2 . . ?
C12 C13 C14 121.7(3) . . ?
C12 C13 H13 119.2 . . ?
C40 C35 C32 122.1(4) . . ?
C36 C35 C32 119.5(3) . . ?
C36 C35 C40 118.2(3) . . ?
C1 C2 C7 120.1(3) . . ?
C1 C2 C3 122.3(3) . . ?
C3 C2 C7 117.6(4) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 C15 121.1(4) . . ?
C19 C20 H20 119.5 . . ?
C2 C3 H3 119.2 . . ?
C4 C3 C2 121.5(4) . . ?
C4 C3 H3 119.2 . . ?
C37 C38 C8 119.6(4) . 3_666 ?
C39 C38 C8 122.0(3) . 3_666 ?
C39 C38 C37 118.4(3) . . ?
C34 C29 C28 120.0(4) . . ?
C30 C29 C28 121.8(4) . . ?
C30 C29 C34 117.9(4) . . ?
C24 C27 C28 115.7(3) . . ?
C48 C27 C28 121.8(4) . . ?
C48 C27 C24 122.3(4) . . ?
C33 C32 C35 120.1(3) . . ?
C31 C32 C35 122.0(4) . . ?
C31 C32 C33 117.6(4) . . ?
C9 C10 H10 119.1 . . ?
C11 C10 C9 121.9(3) . . ?
C11 C10 H10 119.1 . . ?
C21 C26 H26 119.4 . . ?
C25 C26 C21 121.2(4) . . ?
C25 C26 H26 119.4 . . ?
C38 C37 H37 119.7 . . ?
C38 C37 C36 120.6(4) . . ?
C36 C37 H37 119.7 . . ?
C13 C12 H12 119.9 . . ?
C13 C12 C11 120.3(4) . . ?
C11 C12 H12 119.9 . . ?
C29 C28 C27 114.5(3) . . ?
C41 C28 C29 122.8(4) . . ?
C41 C28 C27 122.7(4) . . ?
C29 C34 H34 119.4 . . ?
C33 C34 C29 121.2(4) . . ?
C33 C34 H34 119.4 . . ?
C35 C40 H40 119.6 . . ?
C39 C40 C35 120.8(4) . . ?
C39 C40 H40 119.6 . . ?
C26 C25 H25 119.6 . . ?
C26 C25 C24 120.7(4) . . ?
C24 C25 H25 119.6 . . ?
C25 C24 C27 121.6(4) . . ?
C23 C24 C27 120.4(4) . . ?
C23 C24 C25 117.8(4) . . ?
C32 C33 H33 119.4 . . ?
C34 C33 C32 121.1(4) . . ?
C34 C33 H33 119.4 . . ?
C38 C39 C40 121.2(4) . . ?
C38 C39 H39 119.4 . . ?
C40 C39 H39 119.4 . . ?
C32 C31 H31 119.7 . . ?
C30 C31 C32 120.7(4) . . ?
C30 C31 H31 119.7 . . ?
C29 C30 H30 119.4 . . ?
C31 C30 C29 121.3(4) . . ?
C31 C30 H30 119.4 . . ?
C35 C36 C37 120.8(4) . . ?
C35 C36 H36 119.6 . . ?
C37 C36 H36 119.6 . . ?
C7 C6 H6 119.2 . . ?
C5 C6 C7 121.6(4) . . ?
C5 C6 H6 119.2 . . ?
C24 C23 H23 119.1 . . ?
C22 C23 C24 121.7(4) . . ?
C22 C23 H23 119.1 . . ?
C10 C11 C12 119.9(4) . . ?
C10 C11 H11 120.0 . . ?
C12 C11 H11 120.0 . . ?
C21 C22 H22 119.6 . . ?
C23 C22 C21 120.8(4) . . ?
C23 C22 H22 119.6 . . ?
C18 C17 H17 119.3 . . ?
C16 C17 C18 121.4(4) . . ?
C16 C17 H17 119.3 . . ?
C15 C16 H16 119.5 . . ?
C17 C16 C15 121.1(4) . . ?
C17 C16 H16 119.5 . . ?
C6 C5 H5 120.0 . . ?
C6 C5 C4 120.0(4) . . ?
C4 C5 H5 120.0 . . ?
Si2 C48 H48 113.8 . . ?
C27 C48 Si2 132.4(3) . . ?
C27 C48 H48 113.8 . . ?
C3 C4 C5 120.6(4) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
Si1 C41 H41 114.4 . . ?
C28 C41 Si1 131.1(3) . . ?
C28 C41 H41 114.4 . . ?
C61 O1 C58 106.7(5) . . ?
Si2 C49 H49A 109.5 . . ?
Si2 C49 H49B 109.5 . . ?
Si2 C49 H49C 109.5 . . ?
H49A C49 H49B 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
H60A C60 H60B 109.0 . . ?
C61 C60 H60A 111.1 . . ?
C61 C60 H60B 111.1 . . ?
C61 C60 C59 103.5(5) . . ?
C59 C60 H60A 111.1 . . ?
C59 C60 H60B 111.1 . . ?
Si1 C43 H43A 109.5 . . ?
Si1 C43 H43B 109.5 . . ?
Si1 C43 H43C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O1 C61 C60 110.4(5) . . ?
O1 C61 H61A 109.6 . . ?
O1 C61 H61B 109.6 . . ?
C60 C61 H61A 109.6 . . ?
C60 C61 H61B 109.6 . . ?
H61A C61 H61B 108.1 . . ?
Si2 C50 H50A 109.5 . . ?
Si2 C50 H50B 109.5 . . ?
Si2 C50 H50C 109.5 . . ?
H50A C50 H50B 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
O1 C58 H58A 110.5 . . ?
O1 C58 H58B 110.5 . . ?
O1 C58 C59 106.3(6) . . ?
H58A C58 H58B 108.7 . . ?
C59 C58 H58A 110.5 . . ?
C59 C58 H58B 110.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
Si1 C42 H42A 109.5 . . ?
Si1 C42 H42B 109.5 . . ?
Si1 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C60 C59 H59A 111.5 . . ?
C60 C59 H59B 111.5 . . ?
C58 C59 C60 101.3(5) . . ?
C58 C59 H59A 111.5 . . ?
C58 C59 H59B 111.5 . . ?
H59A C59 H59B 109.3 . . ?
Si1 C44 H44A 107.9 . . ?
Si1 C44 H44B 107.9 . . ?
H44A C44 H44B 107.2 . . ?
C45 C44 Si1 117.4(7) . . ?
C45 C44 H44A 107.9 . . ?
C45 C44 H44B 107.9 . . ?
C44 C45 H45A 108.2 . . ?
C44 C45 H45B 108.2 . . ?
C44 C45 C46 116.5(9) . . ?
H45A C45 H45B 107.3 . . ?
C46 C45 H45A 108.2 . . ?
C46 C45 H45B 108.2 . . ?
C47 C46 H46A 108.6 . . ?
C47 C46 H46B 108.6 . . ?
C45 C46 C47 114.7(8) . . ?
C45 C46 H46A 108.6 . . ?
C45 C46 H46B 108.6 . . ?
H46A C46 H46B 107.6 . . ?
Si2 C51 H51A 107.3 . . ?
Si2 C51 H51B 107.3 . . ?
Si2 C51 H51C 111.2 . . ?
Si2 C51 H51D 111.2 . . ?
H51A C51 H51B 106.9 . . ?
H51C C51 H51D 109.1 . . ?
C55 C51 Si2 120.1(9) . . ?
C55 C51 H51A 107.3 . . ?
C55 C51 H51B 107.3 . . ?
C52 C51 Si2 102.9(8) . . ?
C52 C51 H51C 111.2 . . ?
C52 C51 H51D 111.2 . . ?
H53A C53 H53B 105.7 . . ?
C52 C53 H53A 104.6 . . ?
C52 C53 H53B 104.6 . . ?
C52 C53 C57 130.7(18) . . ?
C57 C53 H53A 104.6 . . ?
C57 C53 H53B 104.6 . . ?
C51 C55 H55A 106.9 . . ?
C51 C55 H55B 106.9 . . ?
C51 C55 C56 121.6(14) . . ?
H55A C55 H55B 106.7 . . ?
C56 C55 H55A 106.9 . . ?
C56 C55 H55B 106.9 . . ?
C51 C52 H52A 110.3 . . ?
C51 C52 H52B 110.3 . . ?
C53 C52 C51 107.1(13) . . ?
C53 C52 H52A 110.3 . . ?
C53 C52 H52B 110.3 . . ?
H52A C52 H52B 108.5 . . ?
C53 C57 H57A 109.5 . . ?
C53 C57 H57B 109.5 . . ?
C53 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
H54A C54 H54B 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C56 C54 H54A 109.5 . . ?
C56 C54 H54B 109.5 . . ?
C56 C54 H54C 109.5 . . ?
C55 C56 H56A 115.7 . . ?
C55 C56 H56B 115.7 . . ?
C54 C56 C55 77.0(14) . . ?
C54 C56 H56A 115.7 . . ?
C54 C56 H56B 115.7 . . ?
H56A C56 H56B 112.7 . . ?
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
Si2 C48 1.870(5) . ?
Si2 C49 1.869(5) . ?
Si2 C50 1.858(6) . ?
Si2 C51 1.835(8) . ?
Si1 C41 1.866(5) . ?
Si1 C43 1.859(5) . ?
Si1 C42 1.839(7) . ?
Si1 C44 1.864(8) . ?
C14 C9 1.439(5) . ?
C14 C1 1.405(5) . ?
C14 C13 1.424(5) . ?
C9 C8 1.398(5) . ?
C9 C10 1.433(5) . ?
C15 C1 1.495(5) . ?
C15 C20 1.400(5) . ?
C15 C16 1.384(6) . ?
C1 C2 1.406(6) . ?
C19 H19 0.9500 . ?
C19 C18 1.387(6) . ?
C19 C20 1.396(5) . ?
C8 C7 1.414(6) . ?
C8 C38 1.507(5) 3_666 ?
C18 C21 1.487(5) . ?
C18 C17 1.402(6) . ?
C7 C2 1.445(5) . ?
C7 C6 1.425(6) . ?
C21 C26 1.400(6) . ?
C21 C22 1.398(6) . ?
C13 H13 0.9500 . ?
C13 C12 1.357(6) . ?
C35 C32 1.491(5) . ?
C35 C40 1.394(6) . ?
C35 C36 1.384(6) . ?
C2 C3 1.432(6) . ?
C20 H20 0.9500 . ?
C3 H3 0.9500 . ?
C3 C4 1.359(6) . ?
C38 C8 1.507(5) 3_666 ?
C38 C37 1.388(6) . ?
C38 C39 1.381(6) . ?
C29 C28 1.497(5) . ?
C29 C34 1.391(6) . ?
C29 C30 1.388(6) . ?
C27 C28 1.504(6) . ?
C27 C24 1.497(6) . ?
C27 C48 1.342(6) . ?
C32 C33 1.401(6) . ?
C32 C31 1.396(6) . ?
C10 H10 0.9500 . ?
C10 C11 1.354(6) . ?
C26 H26 0.9500 . ?
C26 C25 1.390(6) . ?
C37 H37 0.9500 . ?
C37 C36 1.397(5) . ?
C12 H12 0.9500 . ?
C12 C11 1.425(6) . ?
C28 C41 1.345(6) . ?
C34 H34 0.9500 . ?
C34 C33 1.374(5) . ?
C40 H40 0.9500 . ?
C40 C39 1.382(5) . ?
C25 H25 0.9500 . ?
C25 C24 1.401(6) . ?
C24 C23 1.387(6) . ?
C33 H33 0.9500 . ?
C39 H39 0.9500 . ?
C31 H31 0.9500 . ?
C31 C30 1.387(6) . ?
C30 H30 0.9500 . ?
C36 H36 0.9500 . ?
C6 H6 0.9500 . ?
C6 C5 1.359(6) . ?
C23 H23 0.9500 . ?
C23 C22 1.385(6) . ?
C11 H11 0.9500 . ?
C22 H22 0.9500 . ?
C17 H17 0.9500 . ?
C17 C16 1.383(6) . ?
C16 H16 0.9500 . ?
C5 H5 0.9500 . ?
C5 C4 1.419(6) . ?
C48 H48 0.9500 . ?
C4 H4 0.9500 . ?
C41 H41 0.9500 . ?
O1 C61 1.384(7) . ?
O1 C58 1.440(7) . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C60 H60A 0.9900 . ?
C60 H60B 0.9900 . ?
C60 C61 1.463(8) . ?
C60 C59 1.587(10) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C61 H61A 0.9900 . ?
C61 H61B 0.9900 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C58 H58A 0.9900 . ?
C58 H58B 0.9900 . ?
C58 C59 1.469(9) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C47 C46 1.613(14) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C45 1.406(13) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C45 C46 1.568(13) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C51 H51C 0.9900 . ?
C51 H51D 0.9900 . ?
C51 C55 1.49(2) . ?
C51 C52 1.667(18) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C52 1.57(2) . ?
C53 C57 1.65(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C56 1.79(3) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C54 C56 1.52(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
