# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2017
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
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data_5
_database_code_depnum_ccdc_archive 'CCDC 1547176'
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_refine_special_details
;
The triisopropylsilyl group centred at Si1 is disordered over two orientations.
The occupancies of the two were allowed to freely refine, converging at a final
ratio of 0.65:0.35. Chemically equivalent 1,2 N-Si, Si-C and C-C distances
within the disordered groups were restrained to be approximately equal.
The lattice toluene molecule is disordered over an inversion centre.
Aromatic C-C distances within the toluene were restrained to be approximately 1.39 A
and the C-Cmethyl bond distance restrained to approximately 1.55 A
Chemically equivalent 1,3 and 1,4 C-C distances within the toluene were restrained to
be approximately equal and the toluene was restrained to be approximately flat.
Enhanced rigid bond, and similarity thermal restraints were applied to each set of atoms within disordered components to aid refinement.
Selected atoms in disordered components were refined isotropically.
;
_vrf_PLAT201_5
;
PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 1 Report
RESPONSE: Selected atoms in disordered components
were refined isotropically to aid refinement.
;
_vrf_PLAT213_5
;
PROBLEM: Atom C11 has ADP max/min Ratio ..... 4.2 prolat
RESPONSE: No obvious disorder is present at the atom site.
Attempts to restrain the Tren backbone atoms did not
lead to a more acceptable ADP ratio so this was left as is.
;
_audit_creation_date 2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C66 H150 N8 Se Si6 U2, C7 H8'
_chemical_formula_sum 'C73 H158 N8 Se Si6 U2'
_chemical_formula_weight 1871.62
_chemical_melting_point ?
_chemical_oxdiff_formula 'C66 H150 N8 Se1 Si6 U2'
_chemical_oxdiff_usercomment
'UBMGMZ #12223 for BMG/STL in fomblin oil on micromount'
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'
Se Se -0.7943 1.1372 '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'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 25.2002(16)
_cell_length_b 19.5179(10)
_cell_length_c 17.5099(9)
_cell_angle_alpha 90
_cell_angle_beta 98.942(6)
_cell_angle_gamma 90
_cell_volume 8507.6(8)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 6591
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 74.3240
_cell_measurement_theta_min 4.4960
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 12.242
_exptl_absorpt_correction_T_max 0.925
_exptl_absorpt_correction_T_min 0.587
_exptl_absorpt_correction_type gaussian
_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)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour orange
_exptl_crystal_colour_primary orange
_exptl_crystal_density_diffrn 1.461
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 3816
_exptl_crystal_size_max 0.2777
_exptl_crystal_size_mid 0.2309
_exptl_crystal_size_min 0.1102
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0319
_diffrn_reflns_av_unetI/netI 0.0351
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max 29
_diffrn_reflns_limit_h_min -25
_diffrn_reflns_limit_k_max 23
_diffrn_reflns_limit_k_min -23
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -16
_diffrn_reflns_number 19074
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full 66.598
_diffrn_reflns_theta_max 66.598
_diffrn_reflns_theta_min 3.551
_diffrn_ambient_temperature 120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -112.00 18.00 2.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- -43.7877 0.0000 -90.0000 65
#__ type_ start__ end____ width___ exp.time_
2 omega -62.00 12.00 2.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- -43.7877 38.0000 -30.0000 37
#__ type_ start__ end____ width___ exp.time_
3 omega 43.00 71.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -45.0000 -90.0000 14
#__ type_ start__ end____ width___ exp.time_
4 omega 37.00 67.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 60.0000 15
#__ type_ start__ end____ width___ exp.time_
5 omega 33.00 63.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 -120.0000 15
#__ type_ start__ end____ width___ exp.time_
6 omega 28.00 108.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -95.0000 -150.0000 40
#__ type_ start__ end____ width___ exp.time_
7 omega 40.00 66.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 -60.0000 13
#__ type_ start__ end____ width___ exp.time_
8 omega 33.00 59.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 90.0000 13
#__ type_ start__ end____ width___ exp.time_
9 omega 33.00 65.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 -150.0000 16
#__ type_ start__ end____ width___ exp.time_
10 omega 36.00 62.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -30.0000 30.0000 13
#__ type_ start__ end____ width___ exp.time_
11 omega 36.00 80.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -125.0000 30.0000 22
#__ type_ start__ end____ width___ exp.time_
12 omega 39.00 65.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -45.0000 120.0000 13
#__ type_ start__ end____ width___ exp.time_
13 omega 45.00 91.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -95.0000 -60.0000 23
#__ type_ start__ end____ width___ exp.time_
14 omega 31.00 153.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 0.0000 -150.0000 61
#__ type_ start__ end____ width___ exp.time_
15 omega 37.00 77.00 2.0000 3.0000
omega____ theta____ kappa____ phi______ frames
- 105.8472 -45.0000 -150.0000 20
;
_diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 0.0525701000
_diffrn_orient_matrix_UB_12 -0.0201895000
_diffrn_orient_matrix_UB_13 -0.0286329000
_diffrn_orient_matrix_UB_21 0.0001519000
_diffrn_orient_matrix_UB_22 0.0691554000
_diffrn_orient_matrix_UB_23 -0.0424426000
_diffrn_orient_matrix_UB_31 0.0325423000
_diffrn_orient_matrix_UB_32 0.0323086000
_diffrn_orient_matrix_UB_33 0.0729646000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'SuperNova (Cu) X-ray Source'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7013
_reflns_number_total 7505
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 67.13
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_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 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-2012 (Sheldrick, 2012)'
_refine_diff_density_max 2.108
_refine_diff_density_min -2.193
_refine_diff_density_rms 0.146
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.051
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 499
_refine_ls_number_reflns 7505
_refine_ls_number_restraints 409
_refine_ls_R_factor_all 0.0356
_refine_ls_R_factor_gt 0.0331
_refine_ls_restrained_S_all 1.107
_refine_ls_shift/su_max 0.003
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+62.1143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0819
_refine_ls_wR_factor_ref 0.0834
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C1H-C1G = C1H-C1C = C1D-C1C = C1E-C1D = C1F-C1E = C1G-C1F
1.39 with sigma of 0.01
C1C-C1B
1.55 with sigma of 0.02
C1F-C1C \\sim C1E-C1H \\sim C1D-C1G
with sigma of 0.01
C1H-C1B \\sim C1B-C1D
with sigma of 0.01
C1F-C1H \\sim C1H-C1D \\sim C1G-C1E \\sim C1E-C1C
with sigma of 0.01
Si1A-N1 \\sim Si1-N1 \\sim Si2-N2 \\sim Si3-N3
with sigma of 0.003
C2-C1 \\sim C3-C1 \\sim C2A-C1A \\sim C3A-C1A \\sim C5-C4 \\sim C6-C4 \\sim
C5A-C4A \\sim C6A-C4A \\sim C8-C7
\\sim C9-C7 \\sim C8A-C7A \\sim C9A-C7A
with sigma of 0.02
Si1A-C7A \\sim Si1-C7 \\sim Si1A-C4A \\sim Si1-C4 \\sim Si1-C1 \\sim Si1A-C1A
with sigma of 0.02
3. Restrained planarity
C1B, C1C, C1D, C1H, C1E, C1G, C1F
with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1C \\sim C1B \\sim C1D \\sim C1H \\sim C1E \\sim C1G \\sim C1F: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Si1 \\sim Si1A \\sim C2 \\sim C1 \\sim C3 \\sim C4 \\sim C6 \\sim C7 \\sim C9
\\sim C8 \\sim C5 \\sim C7A \\sim C4A \\sim C5A \\sim C8A \\sim C9A \\sim C6A
\\sim C2A \\sim C1A \\sim C3A \\sim N1: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
5. Rigid body (RIGU) restrains
C1C, C1B, C1D, C1H, C1E, C1G, C1F, Si1, Si1A, C2, C1, C3, C4, C6, C7, C9, C8,
C5, C7A, C4A, C5A, C8A, C9A, C6A, C2A, C1A, C3A, N1
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6. Others
Sof(Si1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3A)=
Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C6)=Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=
Sof(H7)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=1-FVAR(1)
Sof(Si1A)=Sof(C7A)=Sof(H7A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
Sof(H5AC)=Sof(C8A)=Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=
Sof(H9AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=
Sof(H2AC)=Sof(C1A)=Sof(H1A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=FVAR(1)
Fixed Sof: C1B(0.5) H1BA(0.5) H1BB(0.5) H1BC(0.5) C1C(0.5) C1D(0.5) H1D(0.5)
C1E(0.5) H1E(0.5) C1F(0.5) H1F(0.5) C1G(0.5) H1G(0.5) C1H(0.5) H1H(0.5)
7.a Ternary CH refined with riding coordinates:
C12(H12), C15(H15), C18(H18), C23(H23), C26(H26), C29(H29), C1(H1), C4(H4),
C7(H7), C7A(H7A), C4A(H4A), C1A(H1A)
7.b Secondary CH2 refined with riding coordinates:
C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
H32B), C33(H33A,H33B)
7.c Aromatic/amide H refined with riding coordinates:
C1D(H1D), C1E(H1E), C1F(H1F), C1G(H1G), C1H(H1H)
7.d Idealised Me refined as rotating group:
C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C17(H17A,H17B,
H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C24(H24A,H24B,H24C), C25(H25A,
H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,H30C),
C31(H31A,H31B,H31C), C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C6(H6A,H6B,H6C), C9(H9A,
H9B,H9C), C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C8A(H8AA,H8AB,
H8AC), C9A(H9AA,H9AB,H9AC), C6A(H6AA,H6AB,H6AC), C2A(H2AA,H2AB,H2AC), C3A(H3AA,
H3AB,H3AC), C1B(H1BA,H1BB,H1BC)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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
U1 U 0.38919(2) 0.71128(2) 0.25519(2) 0.00944(7) Uani 1 1 d . . . . .
Se1 Se 0.500000 0.71684(4) 0.250000 0.01441(15) Uani 1 2 d S T P . .
C10 C 0.3184(2) 0.5961(3) 0.3057(3) 0.0312(14) Uani 1 1 d . . . . .
H10A H 0.309038 0.547426 0.311964 0.037 Uiso 1 1 calc R . . . .
H10B H 0.331191 0.615323 0.357597 0.037 Uiso 1 1 calc R . . . .
C11 C 0.2695(2) 0.6344(3) 0.2691(4) 0.0369(16) Uani 1 1 d . . . . .
H11A H 0.256447 0.615505 0.217131 0.044 Uiso 1 1 calc R . . . .
H11B H 0.240583 0.629680 0.301028 0.044 Uiso 1 1 calc R . . . .
N2 N 0.37294(14) 0.7653(2) 0.36335(18) 0.0139(8) Uani 1 1 d D . . . .
Si2 Si 0.41092(5) 0.77911(6) 0.45399(7) 0.0116(2) Uani 1 1 d D . . . .
C12 C 0.4667(2) 0.7126(2) 0.4683(3) 0.0139(10) Uani 1 1 d . . . . .
H12 H 0.495993 0.730133 0.440970 0.017 Uiso 1 1 calc R . . . .
C13 C 0.4503(2) 0.6421(3) 0.4333(3) 0.0174(10) Uani 1 1 d . . . . .
H13A H 0.415765 0.628475 0.447885 0.026 Uiso 1 1 calc GR . . . .
H13B H 0.477724 0.608141 0.452794 0.026 Uiso 1 1 calc GR . . . .
H13C H 0.446794 0.644599 0.376825 0.026 Uiso 1 1 calc GR . . . .
C14 C 0.4917(2) 0.7023(3) 0.5537(3) 0.0195(11) Uani 1 1 d . . . . .
H14A H 0.499386 0.747008 0.578353 0.029 Uiso 1 1 calc GR . . . .
H14B H 0.525194 0.676163 0.556365 0.029 Uiso 1 1 calc GR . . . .
H14C H 0.466517 0.677066 0.580563 0.029 Uiso 1 1 calc GR . . . .
C15 C 0.3725(2) 0.7707(3) 0.5390(3) 0.0213(11) Uani 1 1 d . . . . .
H15 H 0.401098 0.771313 0.585415 0.026 Uiso 1 1 calc R . . . .
C16 C 0.3445(3) 0.7007(3) 0.5437(4) 0.0313(14) Uani 1 1 d . . . . .
H16A H 0.314397 0.696818 0.501232 0.047 Uiso 1 1 calc GR . . . .
H16B H 0.331151 0.697122 0.593217 0.047 Uiso 1 1 calc GR . . . .
H16C H 0.370320 0.663792 0.539754 0.047 Uiso 1 1 calc GR . . . .
C17 C 0.3342(3) 0.8279(3) 0.5542(4) 0.0342(14) Uani 1 1 d . . . . .
H17A H 0.351633 0.872341 0.550016 0.051 Uiso 1 1 calc GR . . . .
H17B H 0.325110 0.822688 0.606277 0.051 Uiso 1 1 calc GR . . . .
H17C H 0.301427 0.825363 0.516063 0.051 Uiso 1 1 calc GR . . . .
C18 C 0.4434(2) 0.8675(3) 0.4586(3) 0.0184(10) Uani 1 1 d . . . . .
H18 H 0.470891 0.865146 0.423180 0.022 Uiso 1 1 calc R . . . .
C19 C 0.4744(2) 0.8868(3) 0.5376(3) 0.0270(12) Uani 1 1 d . . . . .
H19A H 0.449660 0.888299 0.575645 0.040 Uiso 1 1 calc GR . . . .
H19B H 0.490986 0.931907 0.534506 0.040 Uiso 1 1 calc GR . . . .
H19C H 0.502380 0.852577 0.553529 0.040 Uiso 1 1 calc GR . . . .
C20 C 0.4061(2) 0.9267(3) 0.4282(3) 0.0252(12) Uani 1 1 d . . . . .
H20A H 0.386021 0.914442 0.377573 0.038 Uiso 1 1 calc GR . . . .
H20B H 0.427527 0.967866 0.423254 0.038 Uiso 1 1 calc GR . . . .
H20C H 0.380921 0.935547 0.464451 0.038 Uiso 1 1 calc GR . . . .
C21 C 0.3198(2) 0.8001(3) 0.3498(3) 0.0224(11) Uani 1 1 d . . . . .
H21A H 0.318189 0.832001 0.305548 0.027 Uiso 1 1 calc R . . . .
H21B H 0.314692 0.826862 0.396090 0.027 Uiso 1 1 calc R . . . .
C22 C 0.2760(2) 0.7468(4) 0.3329(3) 0.0303(14) Uani 1 1 d . . . . .
H22A H 0.277231 0.715412 0.377516 0.036 Uiso 1 1 calc R . . . .
H22B H 0.240434 0.769489 0.324293 0.036 Uiso 1 1 calc R . . . .
N3 N 0.34257(15) 0.76733(17) 0.1536(2) 0.0122(8) Uani 1 1 d D . . . .
Si3 Si 0.34941(5) 0.84490(6) 0.10691(7) 0.0107(2) Uani 1 1 d D . . . .
C23 C 0.41808(18) 0.8779(2) 0.1501(3) 0.0125(9) Uani 1 1 d . . . . .
H23 H 0.443821 0.839207 0.148204 0.015 Uiso 1 1 calc R . . . .
C24 C 0.4199(2) 0.8962(3) 0.2363(3) 0.0197(11) Uani 1 1 d . . . . .
H24A H 0.397732 0.936861 0.240724 0.030 Uiso 1 1 calc GR . . . .
H24B H 0.457034 0.905632 0.259756 0.030 Uiso 1 1 calc GR . . . .
H24C H 0.405949 0.857669 0.263167 0.030 Uiso 1 1 calc GR . . . .
C25 C 0.43959(19) 0.9387(3) 0.1080(3) 0.0174(10) Uani 1 1 d . . . . .
H25A H 0.440147 0.926286 0.053844 0.026 Uiso 1 1 calc GR . . . .
H25B H 0.476090 0.949842 0.132964 0.026 Uiso 1 1 calc GR . . . .
H25C H 0.416222 0.978505 0.110203 0.026 Uiso 1 1 calc GR . . . .
C26 C 0.34275(18) 0.8289(3) -0.0012(3) 0.0146(10) Uani 1 1 d . . . . .
H26 H 0.307174 0.805995 -0.016491 0.017 Uiso 1 1 calc R . . . .
C27 C 0.3850(3) 0.7778(3) -0.0200(3) 0.0311(14) Uani 1 1 d . . . . .
H27A H 0.420999 0.796834 -0.003780 0.047 Uiso 1 1 calc GR . . . .
H27B H 0.379657 0.769152 -0.075848 0.047 Uiso 1 1 calc GR . . . .
H27C H 0.381499 0.734701 0.007460 0.047 Uiso 1 1 calc GR . . . .
C28 C 0.3422(2) 0.8927(3) -0.0534(3) 0.0205(11) Uani 1 1 d . . . . .
H28A H 0.317847 0.927196 -0.037320 0.031 Uiso 1 1 calc GR . . . .
H28B H 0.329742 0.879766 -0.107269 0.031 Uiso 1 1 calc GR . . . .
H28C H 0.378504 0.911772 -0.048670 0.031 Uiso 1 1 calc GR . . . .
C29 C 0.29372(19) 0.9073(3) 0.1251(3) 0.0168(10) Uani 1 1 d . . . . .
H29 H 0.289141 0.900759 0.180390 0.020 Uiso 1 1 calc R . . . .
C30 C 0.3070(2) 0.9840(3) 0.1167(4) 0.0264(12) Uani 1 1 d . . . . .
H30A H 0.338743 0.995961 0.154088 0.040 Uiso 1 1 calc GR . . . .
H30B H 0.276435 1.011894 0.126337 0.040 Uiso 1 1 calc GR . . . .
H30C H 0.314329 0.992685 0.064157 0.040 Uiso 1 1 calc GR . . . .
C31 C 0.2388(2) 0.8920(3) 0.0771(3) 0.0251(12) Uani 1 1 d . . . . .
H31A H 0.241087 0.897389 0.022016 0.038 Uiso 1 1 calc GR . . . .
H31B H 0.212026 0.923921 0.091486 0.038 Uiso 1 1 calc GR . . . .
H31C H 0.228213 0.844909 0.086931 0.038 Uiso 1 1 calc GR . . . .
C32 C 0.2905(2) 0.7311(3) 0.1294(3) 0.0205(11) Uani 1 1 d . . . . .
H32A H 0.297205 0.681844 0.121239 0.025 Uiso 1 1 calc R . . . .
H32B H 0.272113 0.750488 0.080009 0.025 Uiso 1 1 calc R . . . .
C33 C 0.2556(2) 0.7393(3) 0.1910(3) 0.0265(13) Uani 1 1 d . . . . .
H33A H 0.249218 0.788543 0.199855 0.032 Uiso 1 1 calc R . . . .
H33B H 0.220464 0.716786 0.174797 0.032 Uiso 1 1 calc R . . . .
N4 N 0.28374(17) 0.7073(2) 0.2628(3) 0.0235(11) Uani 1 1 d . . . . .
Si1 Si 0.38381(12) 0.52590(10) 0.21275(12) 0.0117(5) Uiso 0.648(5) 1 d D U . A
2
Si1A Si 0.35594(18) 0.52781(15) 0.20259(19) 0.0138(10) Uani 0.352(5) 1 d D U .
A 1
C2 C 0.4055(6) 0.6128(7) 0.0874(9) 0.019(3) Uani 0.648(5) 1 d D U . A 2
H2A H 0.367520 0.605410 0.066923 0.028 Uiso 0.648(5) 1 calc GR . . A 2
H2B H 0.425872 0.618427 0.044473 0.028 Uiso 0.648(5) 1 calc GR . . A 2
H2C H 0.409305 0.654094 0.119621 0.028 Uiso 0.648(5) 1 calc GR . . A 2
C1 C 0.4273(4) 0.5509(5) 0.1363(5) 0.0185(16) Uani 0.648(5) 1 d D U . A 2
H1 H 0.462979 0.564950 0.165204 0.022 Uiso 0.648(5) 1 calc R . . A 2
C3 C 0.4381(7) 0.4915(7) 0.0834(7) 0.022(3) Uani 0.648(5) 1 d D U . A 2
H3A H 0.455757 0.454007 0.114784 0.033 Uiso 0.648(5) 1 calc GR . . A 2
H3B H 0.461367 0.507340 0.047079 0.033 Uiso 0.648(5) 1 calc GR . . A 2
H3C H 0.403966 0.475196 0.054479 0.033 Uiso 0.648(5) 1 calc GR . . A 2
C4 C 0.4283(4) 0.4697(4) 0.2876(5) 0.0190(16) Uani 0.648(5) 1 d D U . A 2
H4 H 0.464676 0.491375 0.294675 0.023 Uiso 0.648(5) 1 calc R . . A 2
C6 C 0.4118(3) 0.4689(4) 0.3676(5) 0.0184(16) Uani 0.648(5) 1 d D U . A 2
H6A H 0.404959 0.515836 0.383295 0.028 Uiso 0.648(5) 1 calc GR . . A 2
H6B H 0.440685 0.448744 0.404723 0.028 Uiso 0.648(5) 1 calc GR . . A 2
H6C H 0.379050 0.441478 0.366253 0.028 Uiso 0.648(5) 1 calc GR . . A 2
C7 C 0.3280(3) 0.4668(4) 0.1635(4) 0.0209(15) Uani 0.648(5) 1 d D U . A 2
H7 H 0.347221 0.427394 0.143711 0.025 Uiso 0.648(5) 1 calc R . . A 2
C9 C 0.2938(4) 0.4973(6) 0.0918(6) 0.027(2) Uani 0.648(5) 1 d D U . A 2
H9A H 0.275046 0.538097 0.106539 0.040 Uiso 0.648(5) 1 calc GR . . A 2
H9B H 0.267401 0.463360 0.068843 0.040 Uiso 0.648(5) 1 calc GR . . A 2
H9C H 0.316994 0.510099 0.054095 0.040 Uiso 0.648(5) 1 calc GR . . A 2
C8 C 0.2912(4) 0.4342(5) 0.2157(5) 0.038(2) Uani 0.648(5) 1 d D U . A 2
H8A H 0.312925 0.418011 0.263595 0.056 Uiso 0.648(5) 1 calc GR . . A 2
H8B H 0.271875 0.395429 0.188735 0.056 Uiso 0.648(5) 1 calc GR . . A 2
H8C H 0.265275 0.468318 0.228050 0.056 Uiso 0.648(5) 1 calc GR . . A 2
C5 C 0.4369(3) 0.3950(4) 0.2623(5) 0.037(2) Uani 0.648(5) 1 d D U . A 2
H5A H 0.402591 0.370352 0.256233 0.055 Uiso 0.648(5) 1 calc GR . . A 2
H5B H 0.462814 0.372214 0.301614 0.055 Uiso 0.648(5) 1 calc GR . . A 2
H5C H 0.450607 0.395223 0.212893 0.055 Uiso 0.648(5) 1 calc GR . . A 2
C7A C 0.2888(4) 0.5129(7) 0.1417(7) 0.015(2) Uani 0.352(5) 1 d D U . A 1
H7A H 0.275052 0.558404 0.121050 0.018 Uiso 0.352(5) 1 calc R . . A 1
C4A C 0.3741(5) 0.4566(5) 0.2782(7) 0.017(2) Uiso 0.352(5) 1 d D U . A 1
H4A H 0.346888 0.458988 0.314039 0.020 Uiso 0.352(5) 1 calc R . . A 1
C5A C 0.3707(7) 0.3848(6) 0.2446(9) 0.026(3) Uani 0.352(5) 1 d D U . A 1
H5AA H 0.333587 0.375130 0.221123 0.039 Uiso 0.352(5) 1 calc GR . . A 1
H5AB H 0.382184 0.351545 0.285740 0.039 Uiso 0.352(5) 1 calc GR . . A 1
H5AC H 0.394199 0.381404 0.205038 0.039 Uiso 0.352(5) 1 calc GR . . A 1
C8A C 0.2921(7) 0.4663(9) 0.0724(9) 0.019(3) Uani 0.352(5) 1 d D U . A 1
H8AA H 0.310157 0.490618 0.034720 0.029 Uiso 0.352(5) 1 calc GR . . A 1
H8AB H 0.255771 0.453412 0.048139 0.029 Uiso 0.352(5) 1 calc GR . . A 1
H8AC H 0.312496 0.424905 0.089803 0.029 Uiso 0.352(5) 1 calc GR . . A 1
C9A C 0.2470(5) 0.4829(7) 0.1868(8) 0.025(3) Uani 0.352(5) 1 d D U . A 1
H9AA H 0.257515 0.436285 0.203442 0.038 Uiso 0.352(5) 1 calc GR . . A 1
H9AB H 0.211905 0.481838 0.153611 0.038 Uiso 0.352(5) 1 calc GR . . A 1
H9AC H 0.244754 0.511461 0.232246 0.038 Uiso 0.352(5) 1 calc GR . . A 1
C6A C 0.4289(7) 0.4716(9) 0.3274(13) 0.028(4) Uani 0.352(5) 1 d D U . A 1
H6AA H 0.457425 0.464938 0.295888 0.042 Uiso 0.352(5) 1 calc GR . . A 1
H6AB H 0.434608 0.440330 0.371707 0.042 Uiso 0.352(5) 1 calc GR . . A 1
H6AC H 0.429613 0.519007 0.345857 0.042 Uiso 0.352(5) 1 calc GR . . A 1
C2A C 0.4326(13) 0.4861(12) 0.1066(13) 0.018(4) Uani 0.352(5) 1 d D U . A 1
H2AA H 0.447205 0.452388 0.145758 0.027 Uiso 0.352(5) 1 calc GR . . A 1
H2AB H 0.460687 0.500153 0.077003 0.027 Uiso 0.352(5) 1 calc GR . . A 1
H2AC H 0.402583 0.465754 0.071693 0.027 Uiso 0.352(5) 1 calc GR . . A 1
C1A C 0.4127(6) 0.5488(10) 0.1464(10) 0.015(3) Uiso 0.352(5) 1 d D U . A 1
H1A H 0.443453 0.567324 0.183640 0.018 Uiso 0.352(5) 1 calc R . . A 1
C3A C 0.3958(12) 0.6037(14) 0.0842(18) 0.016(5) Uiso 0.352(5) 1 d D U . A 1
H3AA H 0.369854 0.583928 0.042496 0.023 Uiso 0.352(5) 1 calc GR . . A 1
H3AB H 0.427457 0.619626 0.063330 0.023 Uiso 0.352(5) 1 calc GR . . A 1
H3AC H 0.379189 0.642343 0.107332 0.023 Uiso 0.352(5) 1 calc GR . . A 1
N1 N 0.36269(17) 0.60104(17) 0.2566(2) 0.0236(10) Uani 1 1 d D U . . .
C1B C -0.0855(7) 0.6803(9) 0.2628(14) 0.096(7) Uiso 0.5 1 d D U . B -1
H1BA H -0.110964 0.656035 0.224165 0.144 Uiso 0.5 1 calc GR . . B -1
H1BB H -0.089891 0.729837 0.255112 0.144 Uiso 0.5 1 calc GR . . B -1
H1BC H -0.092283 0.668189 0.314740 0.144 Uiso 0.5 1 calc GR . . B -1
C1C C -0.0266(4) 0.6593(6) 0.2539(9) 0.082(5) Uiso 0.5 1 d D U . B -1
C1D C -0.0124(5) 0.5926(5) 0.2506(13) 0.065(4) Uiso 0.5 1 d D U . B -1
H1D H -0.038157 0.557670 0.254543 0.078 Uiso 0.5 1 calc R . . B -1
C1E C 0.0395(5) 0.5750(5) 0.2414(14) 0.093(5) Uiso 0.5 1 d D U . B -1
H1E H 0.048877 0.528118 0.237571 0.111 Uiso 0.5 1 calc R . . B -1
C1F C 0.0768(4) 0.6237(6) 0.2378(10) 0.058(4) Uiso 0.5 1 d D U . B -1
H1F H 0.112151 0.610987 0.231203 0.069 Uiso 0.5 1 calc R . . B -1
C1G C 0.0637(5) 0.6932(6) 0.2436(14) 0.085(5) Uiso 0.5 1 d D U . B -1
H1G H 0.090422 0.727672 0.244124 0.102 Uiso 0.5 1 calc R . . B -1
C1H C 0.0112(4) 0.7104(4) 0.2486(11) 0.045(3) Uiso 0.5 1 d D U . B -1
H1H H 0.000887 0.757194 0.248425 0.054 Uiso 0.5 1 calc R . . B -1
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
U1 0.00779(9) 0.00883(10) 0.01187(10) 0.00120(5) 0.00210(6) -0.00293(5)
Se1 0.0107(3) 0.0154(4) 0.0186(4) 0.000 0.0068(3) 0.000
C10 0.033(3) 0.033(3) 0.026(3) 0.017(3) -0.002(2) -0.021(3)
C11 0.022(3) 0.057(4) 0.030(3) 0.020(3) -0.002(2) -0.027(3)
N2 0.0079(18) 0.018(2) 0.017(2) 0.0004(17) 0.0031(15) 0.0032(16)
Si2 0.0106(6) 0.0130(6) 0.0124(6) 0.0000(5) 0.0055(5) 0.0005(5)
C12 0.014(2) 0.013(2) 0.014(2) 0.0004(18) 0.0027(19) -0.0015(18)
C13 0.017(2) 0.017(2) 0.019(2) -0.001(2) 0.0027(19) 0.004(2)
C14 0.020(3) 0.020(3) 0.018(3) 0.002(2) 0.001(2) 0.005(2)
C15 0.023(3) 0.025(3) 0.019(3) 0.001(2) 0.012(2) 0.000(2)
C16 0.035(3) 0.036(3) 0.027(3) 0.005(3) 0.021(3) -0.006(3)
C17 0.035(3) 0.038(3) 0.036(3) -0.002(3) 0.025(3) 0.003(3)
C18 0.020(2) 0.013(2) 0.024(3) -0.004(2) 0.010(2) -0.001(2)
C19 0.029(3) 0.021(3) 0.031(3) -0.010(2) 0.005(2) -0.005(2)
C20 0.033(3) 0.015(3) 0.030(3) -0.001(2) 0.010(2) 0.002(2)
C21 0.013(2) 0.035(3) 0.021(3) 0.006(2) 0.008(2) 0.009(2)
C22 0.008(2) 0.062(4) 0.023(3) 0.011(3) 0.006(2) -0.005(3)
N3 0.0109(18) 0.0123(19) 0.0132(19) 0.0052(16) 0.0012(15) -0.0040(15)
Si3 0.0078(5) 0.0113(6) 0.0133(6) 0.0031(5) 0.0026(4) -0.0004(5)
C23 0.011(2) 0.012(2) 0.015(2) 0.0049(18) 0.0020(18) -0.0023(18)
C24 0.016(2) 0.023(3) 0.019(3) -0.001(2) 0.000(2) -0.007(2)
C25 0.015(2) 0.018(3) 0.019(2) 0.004(2) 0.0035(19) -0.006(2)
C26 0.010(2) 0.019(2) 0.014(2) 0.000(2) 0.0021(18) -0.0036(19)
C27 0.046(4) 0.029(3) 0.021(3) 0.004(2) 0.012(3) 0.015(3)
C28 0.020(2) 0.025(3) 0.017(2) 0.004(2) 0.002(2) 0.001(2)
C29 0.013(2) 0.019(3) 0.019(2) 0.002(2) 0.0057(19) 0.003(2)
C30 0.025(3) 0.017(3) 0.038(3) -0.001(2) 0.009(2) 0.011(2)
C31 0.011(2) 0.035(3) 0.029(3) 0.007(2) 0.005(2) 0.008(2)
C32 0.017(2) 0.022(3) 0.019(3) 0.004(2) -0.005(2) -0.010(2)
C33 0.009(2) 0.042(3) 0.027(3) 0.015(3) -0.003(2) -0.008(2)
N4 0.012(2) 0.038(3) 0.018(2) 0.0119(19) -0.0042(17) -0.0106(18)
Si1A 0.004(2) 0.0168(18) 0.0189(18) 0.0060(14) -0.0029(13) -0.0028(13)
C2 0.026(7) 0.012(5) 0.020(5) 0.003(4) 0.012(4) 0.001(4)
C1 0.022(4) 0.015(3) 0.019(3) 0.002(3) 0.005(3) 0.001(3)
C3 0.022(5) 0.017(4) 0.028(7) -0.004(5) 0.010(5) 0.002(4)
C4 0.024(3) 0.014(3) 0.019(4) 0.006(3) 0.005(3) 0.002(3)
C6 0.025(4) 0.013(4) 0.016(4) 0.006(3) -0.002(3) 0.001(3)
C7 0.020(3) 0.021(3) 0.021(3) 0.002(3) 0.002(3) -0.001(3)
C9 0.016(4) 0.028(5) 0.034(5) 0.001(4) -0.003(4) -0.003(4)
C8 0.040(5) 0.043(5) 0.031(5) -0.007(4) 0.007(4) -0.030(4)
C5 0.061(6) 0.020(4) 0.026(4) 0.003(3) -0.003(4) 0.020(4)
C7A 0.008(4) 0.017(5) 0.020(5) 0.004(4) -0.002(4) -0.005(4)
C5A 0.037(8) 0.012(6) 0.027(7) 0.002(6) 0.001(6) 0.006(6)
C8A 0.017(6) 0.017(7) 0.022(6) -0.002(5) -0.004(5) -0.006(6)
C9A 0.017(6) 0.032(7) 0.028(7) 0.004(6) 0.004(5) -0.013(6)
C6A 0.034(7) 0.024(7) 0.024(8) 0.005(7) -0.002(8) 0.005(6)
C2A 0.020(8) 0.014(7) 0.020(9) -0.002(7) 0.005(8) 0.000(6)
N1 0.032(2) 0.014(2) 0.024(2) 0.0086(17) -0.0003(18) -0.0117(18)
_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
U1 Se1 2.8100(2) . ?
U1 N2 2.259(4) . ?
U1 N3 2.256(3) . ?
U1 N4 2.683(4) . ?
U1 N1 2.254(3) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.496(9) . ?
C10 N1 1.513(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 N4 1.475(8) . ?
N2 Si2 1.742(3) . ?
N2 C21 1.487(6) . ?
Si2 C12 1.902(5) . ?
Si2 C15 1.905(5) . ?
Si2 C18 1.905(5) . ?
C12 H12 1.0000 . ?
C12 C13 1.538(7) . ?
C12 C14 1.542(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.545(8) . ?
C15 C17 1.525(8) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.528(7) . ?
C18 C20 1.530(7) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.512(8) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 N4 1.487(8) . ?
N3 Si3 1.742(3) . ?
N3 C32 1.493(6) . ?
Si3 C23 1.891(5) . ?
Si3 C26 1.901(5) . ?
Si3 C29 1.922(5) . ?
C23 H23 1.0000 . ?
C23 C24 1.544(7) . ?
C23 C25 1.539(6) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.532(7) . ?
C26 C28 1.544(7) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C30 1.546(7) . ?
C29 C31 1.533(7) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.503(8) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 N4 1.483(7) . ?
Si1 C1 1.920(8) . ?
Si1 C4 1.929(8) . ?
Si1 C7 1.917(7) . ?
Si1 N1 1.775(3) . ?
Si1A C7A 1.877(11) . ?
Si1A C4A 1.926(10) . ?
Si1A C1A 1.901(13) . ?
Si1A N1 1.708(3) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C1 1.531(9) . ?
C1 H1 1.0000 . ?
C1 C3 1.535(11) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4 1.0000 . ?
C4 C6 1.521(9) . ?
C4 C5 1.548(10) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C9 1.529(10) . ?
C7 C8 1.538(9) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C7A H7A 1.0000 . ?
C7A C8A 1.531(13) . ?
C7A C9A 1.528(12) . ?
C4A H4A 1.0000 . ?
C4A C5A 1.517(12) . ?
C4A C6A 1.537(13) . ?
C5A H5AA 0.9800 . ?
C5A H5AB 0.9800 . ?
C5A H5AC 0.9800 . ?
C8A H8AA 0.9800 . ?
C8A H8AB 0.9800 . ?
C8A H8AC 0.9800 . ?
C9A H9AA 0.9800 . ?
C9A H9AB 0.9800 . ?
C9A H9AC 0.9800 . ?
C6A H6AA 0.9800 . ?
C6A H6AB 0.9800 . ?
C6A H6AC 0.9800 . ?
C2A H2AA 0.9800 . ?
C2A H2AB 0.9800 . ?
C2A H2AC 0.9800 . ?
C2A C1A 1.529(13) . ?
C1A H1A 1.0000 . ?
C1A C3A 1.540(14) . ?
C3A H3AA 0.9800 . ?
C3A H3AB 0.9800 . ?
C3A H3AC 0.9800 . ?
C1B H1BA 0.9800 . ?
C1B H1BB 0.9800 . ?
C1B H1BC 0.9800 . ?
C1B C1C 1.570(17) . ?
C1C C1D 1.354(8) . ?
C1C C1H 1.393(9) . ?
C1D H1D 0.9500 . ?
C1D C1E 1.387(9) . ?
C1E H1E 0.9500 . ?
C1E C1F 1.344(9) . ?
C1F H1F 0.9500 . ?
C1F C1G 1.403(9) . ?
C1G H1G 0.9500 . ?
C1G C1H 1.381(9) . ?
C1H H1H 0.9500 . ?
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
N2 U1 Se1 108.63(9) . . ?
N2 U1 N4 70.23(14) . . ?
N3 U1 Se1 110.74(9) . . ?
N3 U1 N2 107.13(14) . . ?
N3 U1 N4 69.80(13) . . ?
N4 U1 Se1 178.87(11) . . ?
N1 U1 Se1 109.56(11) . . ?
N1 U1 N2 110.06(15) . . ?
N1 U1 N3 110.66(14) . . ?
N1 U1 N4 70.99(15) . . ?
U1 Se1 U1 175.58(3) 2_655 . ?
H10A C10 H10B 108.1 . . ?
C11 C10 H10A 109.5 . . ?
C11 C10 H10B 109.5 . . ?
C11 C10 N1 110.9(4) . . ?
N1 C10 H10A 109.5 . . ?
N1 C10 H10B 109.5 . . ?
C10 C11 H11A 110.0 . . ?
C10 C11 H11B 110.0 . . ?
H11A C11 H11B 108.3 . . ?
N4 C11 C10 108.7(4) . . ?
N4 C11 H11A 110.0 . . ?
N4 C11 H11B 110.0 . . ?
Si2 N2 U1 133.7(2) . . ?
C21 N2 U1 110.8(3) . . ?
C21 N2 Si2 115.3(3) . . ?
N2 Si2 C12 107.7(2) . . ?
N2 Si2 C15 115.1(2) . . ?
N2 Si2 C18 110.5(2) . . ?
C12 Si2 C15 107.1(2) . . ?
C12 Si2 C18 108.0(2) . . ?
C15 Si2 C18 108.2(2) . . ?
Si2 C12 H12 106.8 . . ?
C13 C12 Si2 114.2(3) . . ?
C13 C12 H12 106.8 . . ?
C13 C12 C14 108.3(4) . . ?
C14 C12 Si2 113.6(3) . . ?
C14 C12 H12 106.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15 104.1 . . ?
C16 C15 Si2 114.2(4) . . ?
C16 C15 H15 104.1 . . ?
C17 C15 Si2 119.0(4) . . ?
C17 C15 H15 104.1 . . ?
C17 C15 C16 109.4(5) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18 105.5 . . ?
C19 C18 Si2 114.6(4) . . ?
C19 C18 H18 105.5 . . ?
C19 C18 C20 109.2(4) . . ?
C20 C18 Si2 115.6(4) . . ?
C20 C18 H18 105.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.8 . . ?
N2 C21 H21B 109.8 . . ?
N2 C21 C22 109.2(5) . . ?
H21A C21 H21B 108.3 . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
C21 C22 H22A 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
N4 C22 C21 109.4(4) . . ?
N4 C22 H22A 109.8 . . ?
N4 C22 H22B 109.8 . . ?
Si3 N3 U1 135.6(2) . . ?
C32 N3 U1 108.8(3) . . ?
C32 N3 Si3 115.1(3) . . ?
N3 Si3 C23 105.04(19) . . ?
N3 Si3 C26 109.0(2) . . ?
N3 Si3 C29 110.2(2) . . ?
C23 Si3 C26 112.9(2) . . ?
C23 Si3 C29 111.3(2) . . ?
C26 Si3 C29 108.4(2) . . ?
Si3 C23 H23 106.7 . . ?
C24 C23 Si3 110.8(3) . . ?
C24 C23 H23 106.7 . . ?
C25 C23 Si3 116.0(3) . . ?
C25 C23 H23 106.7 . . ?
C25 C23 C24 109.4(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si3 C26 H26 106.1 . . ?
C27 C26 Si3 111.4(4) . . ?
C27 C26 H26 106.1 . . ?
C27 C26 C28 110.0(4) . . ?
C28 C26 Si3 116.6(3) . . ?
C28 C26 H26 106.1 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si3 C29 H29 106.0 . . ?
C30 C29 Si3 115.0(3) . . ?
C30 C29 H29 106.0 . . ?
C31 C29 Si3 113.9(4) . . ?
C31 C29 H29 106.0 . . ?
C31 C29 C30 109.1(4) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.8 . . ?
N3 C32 H32B 109.8 . . ?
N3 C32 C33 109.3(4) . . ?
H32A C32 H32B 108.3 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
C32 C33 H33A 110.1 . . ?
C32 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
N4 C33 C32 107.9(4) . . ?
N4 C33 H33A 110.1 . . ?
N4 C33 H33B 110.1 . . ?
C11 N4 U1 106.6(3) . . ?
C11 N4 C22 112.0(5) . . ?
C11 N4 C33 112.4(4) . . ?
C22 N4 U1 106.5(3) . . ?
C33 N4 U1 107.0(3) . . ?
C33 N4 C22 112.0(5) . . ?
C1 Si1 C4 106.5(4) . . ?
C7 Si1 C1 107.3(4) . . ?
C7 Si1 C4 105.8(4) . . ?
N1 Si1 C1 109.5(3) . . ?
N1 Si1 C4 110.9(3) . . ?
N1 Si1 C7 116.3(3) . . ?
C7A Si1A C4A 112.1(6) . . ?
C7A Si1A C1A 115.1(7) . . ?
C1A Si1A C4A 113.2(7) . . ?
N1 Si1A C7A 116.6(5) . . ?
N1 Si1A C4A 103.3(4) . . ?
N1 Si1A C1A 95.1(6) . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
Si1 C1 H1 106.4 . . ?
C2 C1 Si1 113.4(7) . . ?
C2 C1 H1 106.4 . . ?
C2 C1 C3 109.9(10) . . ?
C3 C1 Si1 113.7(7) . . ?
C3 C1 H1 106.4 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4 105.5 . . ?
C6 C4 Si1 114.7(6) . . ?
C6 C4 H4 105.5 . . ?
C6 C4 C5 108.9(7) . . ?
C5 C4 Si1 115.6(6) . . ?
C5 C4 H4 105.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7 104.9 . . ?
C9 C7 Si1 114.6(6) . . ?
C9 C7 H7 104.9 . . ?
C9 C7 C8 109.5(7) . . ?
C8 C7 Si1 116.7(5) . . ?
C8 C7 H7 104.9 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
Si1A C7A H7A 107.4 . . ?
C8A C7A Si1A 112.8(9) . . ?
C8A C7A H7A 107.4 . . ?
C9A C7A Si1A 113.5(9) . . ?
C9A C7A H7A 107.4 . . ?
C9A C7A C8A 108.0(11) . . ?
Si1A C4A H4A 106.5 . . ?
C5A C4A Si1A 114.0(9) . . ?
C5A C4A H4A 106.5 . . ?
C5A C4A C6A 112.6(12) . . ?
C6A C4A Si1A 110.2(10) . . ?
C6A C4A H4A 106.5 . . ?
C4A C5A H5AA 109.5 . . ?
C4A C5A H5AB 109.5 . . ?
C4A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7A C9A H9AA 109.5 . . ?
C7A C9A H9AB 109.5 . . ?
C7A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
C4A C6A H6AA 109.5 . . ?
C4A C6A H6AB 109.5 . . ?
C4A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
C1A C2A H2AC 109.5 . . ?
Si1A C1A H1A 108.1 . . ?
C2A C1A Si1A 112.9(13) . . ?
C2A C1A H1A 108.1 . . ?
C2A C1A C3A 108.0(19) . . ?
C3A C1A Si1A 111.6(15) . . ?
C3A C1A H1A 108.1 . . ?
C1A C3A H3AA 109.5 . . ?
C1A C3A H3AB 109.5 . . ?
C1A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
C10 N1 U1 108.2(3) . . ?
C10 N1 Si1 119.4(3) . . ?
C10 N1 Si1A 104.0(3) . . ?
Si1 N1 U1 132.4(2) . . ?
Si1A N1 U1 142.8(3) . . ?
H1BA C1B H1BB 109.5 . . ?
H1BA C1B H1BC 109.5 . . ?
H1BB C1B H1BC 109.5 . . ?
C1C C1B H1BA 109.5 . . ?
C1C C1B H1BB 109.5 . . ?
C1C C1B H1BC 109.5 . . ?
C1D C1C C1B 121.0(7) . . ?
C1D C1C C1H 119.9(6) . . ?
C1H C1C C1B 119.1(6) . . ?
C1C C1D H1D 119.9 . . ?
C1C C1D C1E 120.2(6) . . ?
C1E C1D H1D 119.9 . . ?
C1D C1E H1E 119.7 . . ?
C1F C1E C1D 120.6(4) . . ?
C1F C1E H1E 119.7 . . ?
C1E C1F H1F 119.8 . . ?
C1E C1F C1G 120.5(6) . . ?
C1G C1F H1F 119.8 . . ?
C1F C1G H1G 120.8 . . ?
C1H C1G C1F 118.4(5) . . ?
C1H C1G H1G 120.8 . . ?
C1C C1H H1H 119.9 . . ?
C1G C1H C1C 120.2(4) . . ?
C1G C1H H1H 119.9 . . ?
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
U1 N2 Si2 C12 -20.7(4) . . . . ?
U1 N2 Si2 C15 -140.0(3) . . . . ?
U1 N2 Si2 C18 97.0(3) . . . . ?
U1 N2 C21 C22 64.5(4) . . . . ?
U1 N3 Si3 C23 9.1(4) . . . . ?
U1 N3 Si3 C26 130.3(3) . . . . ?
U1 N3 Si3 C29 -110.9(3) . . . . ?
U1 N3 C32 C33 68.4(5) . . . . ?
C10 C11 N4 U1 26.7(5) . . . . ?
C10 C11 N4 C22 -89.4(6) . . . . ?
C10 C11 N4 C33 143.6(5) . . . . ?
C11 C10 N1 U1 65.5(5) . . . . ?
C11 C10 N1 Si1 -114.3(5) . . . . ?
C11 C10 N1 Si1A -95.7(5) . . . . ?
N2 C21 C22 N4 -60.0(6) . . . . ?
Si2 N2 C21 C22 -119.9(4) . . . . ?
C21 N2 Si2 C12 165.0(4) . . . . ?
C21 N2 Si2 C15 45.7(4) . . . . ?
C21 N2 Si2 C18 -77.2(4) . . . . ?
C21 C22 N4 U1 27.3(5) . . . . ?
C21 C22 N4 C11 143.4(5) . . . . ?
C21 C22 N4 C33 -89.4(5) . . . . ?
N3 Si3 C23 C24 -66.5(4) . . . . ?
N3 Si3 C23 C25 168.0(4) . . . . ?
N3 C32 C33 N4 -61.6(6) . . . . ?
Si3 N3 C32 C33 -104.6(4) . . . . ?
C26 Si3 C23 C24 175.0(3) . . . . ?
C26 Si3 C23 C25 49.4(4) . . . . ?
C29 Si3 C23 C24 52.8(4) . . . . ?
C29 Si3 C23 C25 -72.8(4) . . . . ?
C32 N3 Si3 C23 179.5(4) . . . . ?
C32 N3 Si3 C26 -59.3(4) . . . . ?
C32 N3 Si3 C29 59.5(4) . . . . ?
C32 C33 N4 U1 26.0(5) . . . . ?
C32 C33 N4 C11 -90.6(5) . . . . ?
C32 C33 N4 C22 142.4(5) . . . . ?
C1 Si1 N1 U1 -13.2(5) . . . . ?
C1 Si1 N1 C10 166.5(4) . . . . ?
C4 Si1 N1 U1 104.1(4) . . . . ?
C4 Si1 N1 C10 -76.2(5) . . . . ?
C7 Si1 N1 U1 -135.0(3) . . . . ?
C7 Si1 N1 C10 44.7(5) . . . . ?
C7A Si1A N1 U1 -92.9(6) . . . . ?
C7A Si1A N1 C10 56.7(6) . . . . ?
C4A Si1A C7A C8A -85.6(11) . . . . ?
C4A Si1A C7A C9A 37.7(12) . . . . ?
C4A Si1A N1 U1 143.7(5) . . . . ?
C4A Si1A N1 C10 -66.7(5) . . . . ?
C1A Si1A C7A C8A 45.6(13) . . . . ?
C1A Si1A C7A C9A 168.8(10) . . . . ?
C1A Si1A N1 U1 28.4(7) . . . . ?
C1A Si1A N1 C10 178.1(6) . . . . ?
N1 C10 C11 N4 -61.2(6) . . . . ?
N1 Si1A C7A C8A 155.7(9) . . . . ?
N1 Si1A C7A C9A -81.1(10) . . . . ?
C1B C1C C1D C1E 178.9(14) . . . . ?
C1B C1C C1H C1G 177.6(17) . . . . ?
C1C C1D C1E C1F 2(3) . . . . ?
C1D C1C C1H C1G -3(3) . . . . ?
C1D C1E C1F C1G 0(3) . . . . ?
C1E C1F C1G C1H -4(3) . . . . ?
C1F C1G C1H C1C 5(3) . . . . ?
C1H C1C C1D C1E 0(2) . . . . ?
_shelx_res_file
;
TITL UBMGMZ in C2/c #15
ubmgmz.res
created by SHELXL-2016/6 at 16:15:43 on 27-Apr-2017
REM reset to C2/c #15
CELL 1.54184 25.20016 19.517856 17.509858 90 98.9415 90
ZERR 4 0.001564 0.000992 0.0009 0 0.006 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N Se Si U
UNIT 292 632 32 4 24 8
DFIX 1.39 0.01 C1H C1G C1H C1C C1D C1C C1E C1D C1F C1E C1G C1F
DFIX 1.55 C1C C1B
SADI 0.01 C1F C1C C1E C1H C1D C1G
SADI 0.01 C1H C1B C1B C1D
SADI 0.01 C1F C1H C1H C1D C1G C1E C1E C1C
SADI 0.003 Si1A N1 Si1 N1 Si2 N2 Si3 N3
SADI C2 C1 C3 C1 C2A C1A C3A C1A C5 C4 C6 C4 C5A C4A C6A C4A C8 C7 C9 C7 C8A =
C7A C9A C7A
SADI Si1A C7A Si1 C7 Si1A C4A Si1 C4 Si1 C1 Si1A C1A
FLAT C1B C1C C1D C1H C1E C1G C1F
SIMU 0.01 0.02 2 C1C C1B C1D C1H C1E C1G C1F
SIMU 0.01 0.02 2 Si1 Si1A C2 C1 C3 C4 C6 C7 C9 C8 C5 C7A C4A C5A C8A C9A C6A =
C2A C1A C3A N1
RIGU C1C C1B C1D C1H C1E C1G C1F Si1 Si1A C2 C1 C3 C4 C6 C7 C9 C8 C5 C7A C4A =
C5A C8A C9A C6A C2A C1A C3A N1
L.S. 32
PLAN 20
TEMP -153(2)
BOND $H
conf
MORE -1
fmap 2
bump
acta
SHEL 100 0.84
REM
REM
REM
WGHT 0.042600 62.114300
FVAR 1.07672 0.35230
U1 6 0.389192 0.711281 0.255188 11.00000 0.00779 0.00883 =
0.01187 0.00120 0.00210 -0.00293
SE1 4 0.500000 0.716839 0.250000 10.50000 0.01070 0.01541 =
0.01858 0.00000 0.00684 0.00000
C10 1 0.318385 0.596148 0.305656 11.00000 0.03267 0.03343 =
0.02551 0.01748 -0.00181 -0.02116
AFIX 23
H10A 2 0.309038 0.547426 0.311964 11.00000 -1.20000
H10B 2 0.331191 0.615323 0.357597 11.00000 -1.20000
AFIX 0
C11 1 0.269533 0.634433 0.269104 11.00000 0.02174 0.05684 =
0.02994 0.02006 -0.00246 -0.02726
AFIX 23
H11A 2 0.256447 0.615505 0.217131 11.00000 -1.20000
H11B 2 0.240583 0.629680 0.301028 11.00000 -1.20000
AFIX 0
N2 3 0.372945 0.765260 0.363346 11.00000 0.00788 0.01755 =
0.01671 0.00043 0.00309 0.00318
SI2 5 0.410923 0.779113 0.453987 11.00000 0.01058 0.01301 =
0.01237 -0.00002 0.00548 0.00050
C12 1 0.466735 0.712606 0.468332 11.00000 0.01449 0.01348 =
0.01389 0.00042 0.00268 -0.00151
AFIX 13
H12 2 0.495993 0.730133 0.440970 11.00000 -1.20000
AFIX 0
C13 1 0.450260 0.642055 0.433279 11.00000 0.01668 0.01670 =
0.01876 -0.00098 0.00268 0.00434
AFIX 137
H13A 2 0.415765 0.628475 0.447885 11.00000 -1.50000
H13B 2 0.477724 0.608141 0.452794 11.00000 -1.50000
H13C 2 0.446794 0.644599 0.376825 11.00000 -1.50000
AFIX 0
C14 1 0.491736 0.702269 0.553682 11.00000 0.01998 0.01957 =
0.01834 0.00241 0.00065 0.00542
AFIX 137
H14A 2 0.499386 0.747008 0.578353 11.00000 -1.50000
H14B 2 0.525194 0.676163 0.556365 11.00000 -1.50000
H14C 2 0.466517 0.677066 0.580563 11.00000 -1.50000
AFIX 0
C15 1 0.372470 0.770682 0.538953 11.00000 0.02300 0.02486 =
0.01875 0.00061 0.01198 0.00037
AFIX 13
H15 2 0.401098 0.771313 0.585415 11.00000 -1.20000
AFIX 0
C16 1 0.344531 0.700708 0.543725 11.00000 0.03531 0.03647 =
0.02741 0.00538 0.02111 -0.00626
AFIX 137
H16A 2 0.314397 0.696818 0.501232 11.00000 -1.50000
H16B 2 0.331151 0.697122 0.593217 11.00000 -1.50000
H16C 2 0.370320 0.663792 0.539754 11.00000 -1.50000
AFIX 0
C17 1 0.334246 0.827877 0.554188 11.00000 0.03502 0.03761 =
0.03621 -0.00182 0.02517 0.00339
AFIX 137
H17A 2 0.351633 0.872341 0.550016 11.00000 -1.50000
H17B 2 0.325110 0.822688 0.606277 11.00000 -1.50000
H17C 2 0.301427 0.825363 0.516063 11.00000 -1.50000
AFIX 0
C18 1 0.443380 0.867497 0.458559 11.00000 0.01988 0.01312 =
0.02450 -0.00393 0.01045 -0.00123
AFIX 13
H18 2 0.470891 0.865146 0.423180 11.00000 -1.20000
AFIX 0
C19 1 0.474380 0.886800 0.537648 11.00000 0.02942 0.02098 =
0.03063 -0.00957 0.00486 -0.00520
AFIX 137
H19A 2 0.449660 0.888299 0.575645 11.00000 -1.50000
H19B 2 0.490986 0.931907 0.534506 11.00000 -1.50000
H19C 2 0.502380 0.852577 0.553529 11.00000 -1.50000
AFIX 0
C20 1 0.406111 0.926657 0.428232 11.00000 0.03260 0.01493 =
0.02955 -0.00086 0.00987 0.00159
AFIX 137
H20A 2 0.386021 0.914442 0.377573 11.00000 -1.50000
H20B 2 0.427527 0.967866 0.423254 11.00000 -1.50000
H20C 2 0.380921 0.935547 0.464451 11.00000 -1.50000
AFIX 0
C21 1 0.319818 0.800072 0.349783 11.00000 0.01274 0.03510 =
0.02121 0.00648 0.00804 0.00937
AFIX 23
H21A 2 0.318189 0.832001 0.305548 11.00000 -1.20000
H21B 2 0.314692 0.826862 0.396090 11.00000 -1.20000
AFIX 0
C22 1 0.276001 0.746803 0.332865 11.00000 0.00790 0.06162 =
0.02259 0.01068 0.00599 -0.00482
AFIX 23
H22A 2 0.277231 0.715412 0.377516 11.00000 -1.20000
H22B 2 0.240434 0.769489 0.324293 11.00000 -1.20000
AFIX 0
N3 3 0.342574 0.767331 0.153631 11.00000 0.01091 0.01228 =
0.01321 0.00523 0.00122 -0.00398
SI3 5 0.349410 0.844899 0.106912 11.00000 0.00779 0.01128 =
0.01333 0.00308 0.00259 -0.00036
C23 1 0.418076 0.877926 0.150138 11.00000 0.01148 0.01158 =
0.01458 0.00492 0.00204 -0.00225
AFIX 13
H23 2 0.443821 0.839207 0.148204 11.00000 -1.20000
AFIX 0
C24 1 0.419861 0.896191 0.236320 11.00000 0.01645 0.02313 =
0.01868 -0.00068 0.00009 -0.00701
AFIX 137
H24A 2 0.397732 0.936861 0.240724 11.00000 -1.50000
H24B 2 0.457034 0.905632 0.259756 11.00000 -1.50000
H24C 2 0.405949 0.857669 0.263167 11.00000 -1.50000
AFIX 0
C25 1 0.439587 0.938655 0.107957 11.00000 0.01543 0.01836 =
0.01865 0.00381 0.00350 -0.00616
AFIX 137
H25A 2 0.440147 0.926286 0.053844 11.00000 -1.50000
H25B 2 0.476090 0.949842 0.132964 11.00000 -1.50000
H25C 2 0.416222 0.978505 0.110203 11.00000 -1.50000
AFIX 0
C26 1 0.342748 0.828873 -0.001224 11.00000 0.01032 0.01927 =
0.01421 -0.00042 0.00211 -0.00360
AFIX 13
H26 2 0.307174 0.805995 -0.016491 11.00000 -1.20000
AFIX 0
C27 1 0.385036 0.777787 -0.020044 11.00000 0.04574 0.02892 =
0.02089 0.00366 0.01234 0.01460
AFIX 137
H27A 2 0.420999 0.796834 -0.003780 11.00000 -1.50000
H27B 2 0.379657 0.769152 -0.075848 11.00000 -1.50000
H27C 2 0.381499 0.734701 0.007460 11.00000 -1.50000
AFIX 0
C28 1 0.342156 0.892733 -0.053384 11.00000 0.01996 0.02464 =
0.01660 0.00419 0.00204 0.00093
AFIX 137
H28A 2 0.317847 0.927196 -0.037320 11.00000 -1.50000
H28B 2 0.329742 0.879766 -0.107269 11.00000 -1.50000
H28C 2 0.378504 0.911772 -0.048670 11.00000 -1.50000
AFIX 0
C29 1 0.293716 0.907320 0.125147 11.00000 0.01329 0.01901 =
0.01900 0.00213 0.00570 0.00304
AFIX 13
H29 2 0.289141 0.900759 0.180390 11.00000 -1.20000
AFIX 0
C30 1 0.307023 0.983977 0.116655 11.00000 0.02485 0.01720 =
0.03822 -0.00079 0.00871 0.01099
AFIX 137
H30A 2 0.338743 0.995961 0.154088 11.00000 -1.50000
H30B 2 0.276435 1.011894 0.126337 11.00000 -1.50000
H30C 2 0.314329 0.992685 0.064157 11.00000 -1.50000
AFIX 0
C31 1 0.238807 0.892003 0.077057 11.00000 0.01115 0.03540 =
0.02927 0.00688 0.00459 0.00829
AFIX 137
H31A 2 0.241087 0.897389 0.022016 11.00000 -1.50000
H31B 2 0.212026 0.923921 0.091486 11.00000 -1.50000
H31C 2 0.228213 0.844909 0.086931 11.00000 -1.50000
AFIX 0
C32 1 0.290505 0.731093 0.129352 11.00000 0.01744 0.02210 =
0.01947 0.00432 -0.00493 -0.00954
AFIX 23
H32A 2 0.297205 0.681844 0.121239 11.00000 -1.20000
H32B 2 0.272113 0.750488 0.080009 11.00000 -1.20000
AFIX 0
C33 1 0.255602 0.739337 0.190986 11.00000 0.00882 0.04197 =
0.02690 0.01512 -0.00292 -0.00805
AFIX 23
H33A 2 0.249218 0.788543 0.199855 11.00000 -1.20000
H33B 2 0.220464 0.716786 0.174797 11.00000 -1.20000
AFIX 0
N4 3 0.283740 0.707304 0.262814 11.00000 0.01171 0.03824 =
0.01836 0.01186 -0.00423 -0.01062
PART 2
SI1 5 0.383814 0.525900 0.212748 -21.00000 0.01173
PART 0
PART 1
SI1A 5 0.355944 0.527813 0.202589 21.00000 0.00400 0.01685 =
0.01892 0.00598 -0.00295 -0.00280
PART 0
PART 2
C2 1 0.405535 0.612777 0.087430 -21.00000 0.02639 0.01199 =
0.02010 0.00299 0.01197 0.00082
AFIX 137
H2A 2 0.367520 0.605410 0.066923 -21.00000 -1.50000
H2B 2 0.425872 0.618427 0.044473 -21.00000 -1.50000
H2C 2 0.409305 0.654094 0.119621 -21.00000 -1.50000
AFIX 0
C1 1 0.427260 0.550915 0.136283 -21.00000 0.02186 0.01500 =
0.01933 0.00158 0.00528 0.00077
AFIX 13
H1 2 0.462979 0.564950 0.165204 -21.00000 -1.20000
AFIX 0
C3 1 0.438064 0.491494 0.083374 -21.00000 0.02207 0.01733 =
0.02843 -0.00362 0.01043 0.00185
AFIX 137
H3A 2 0.455757 0.454007 0.114784 -21.00000 -1.50000
H3B 2 0.461367 0.507340 0.047079 -21.00000 -1.50000
H3C 2 0.403966 0.475196 0.054479 -21.00000 -1.50000
AFIX 0
C4 1 0.428291 0.469685 0.287633 -21.00000 0.02384 0.01438 =
0.01934 0.00593 0.00539 0.00243
AFIX 13
H4 2 0.464676 0.491375 0.294675 -21.00000 -1.20000
AFIX 0
C6 1 0.411777 0.468862 0.367589 -21.00000 0.02468 0.01308 =
0.01580 0.00573 -0.00184 0.00140
AFIX 137
H6A 2 0.404959 0.515836 0.383295 -21.00000 -1.50000
H6B 2 0.440685 0.448744 0.404723 -21.00000 -1.50000
H6C 2 0.379050 0.441478 0.366253 -21.00000 -1.50000
AFIX 0
C7 1 0.327971 0.466825 0.163505 -21.00000 0.01982 0.02134 =
0.02130 0.00214 0.00202 -0.00139
AFIX 13
H7 2 0.347221 0.427394 0.143711 -21.00000 -1.20000
AFIX 0
C9 1 0.293786 0.497332 0.091814 -21.00000 0.01646 0.02802 =
0.03366 0.00054 -0.00312 -0.00311
AFIX 137
H9A 2 0.275046 0.538097 0.106539 -21.00000 -1.50000
H9B 2 0.267401 0.463360 0.068843 -21.00000 -1.50000
H9C 2 0.316994 0.510099 0.054095 -21.00000 -1.50000
AFIX 0
C8 1 0.291175 0.434186 0.215704 -21.00000 0.03972 0.04250 =
0.03125 -0.00717 0.00726 -0.03033
AFIX 137
H8A 2 0.312925 0.418011 0.263595 -21.00000 -1.50000
H8B 2 0.271875 0.395429 0.188735 -21.00000 -1.50000
H8C 2 0.265275 0.468318 0.228050 -21.00000 -1.50000
AFIX 0
C5 1 0.436863 0.395016 0.262265 -21.00000 0.06136 0.01952 =
0.02621 0.00349 -0.00257 0.02007
AFIX 137
H5A 2 0.402591 0.370352 0.256233 -21.00000 -1.50000
H5B 2 0.462814 0.372214 0.301614 -21.00000 -1.50000
H5C 2 0.450607 0.395223 0.212893 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C7A 1 0.288800 0.512927 0.141730 21.00000 0.00754 0.01694 =
0.02005 0.00373 -0.00189 -0.00452
AFIX 13
H7A 2 0.275052 0.558404 0.121050 21.00000 -1.20000
AFIX 0
C4A 1 0.374121 0.456583 0.278233 21.00000 0.01653
AFIX 13
H4A 2 0.346888 0.458988 0.314039 21.00000 -1.20000
AFIX 0
C5A 1 0.370722 0.384813 0.244552 21.00000 0.03670 0.01238 =
0.02703 0.00227 0.00083 0.00603
AFIX 137
H5AA 2 0.333587 0.375130 0.221123 21.00000 -1.50000
H5AB 2 0.382184 0.351545 0.285740 21.00000 -1.50000
H5AC 2 0.394199 0.381404 0.205038 21.00000 -1.50000
AFIX 0
C8A 1 0.292103 0.466269 0.072358 21.00000 0.01722 0.01689 =
0.02192 -0.00241 -0.00360 -0.00645
AFIX 137
H8AA 2 0.310157 0.490618 0.034720 21.00000 -1.50000
H8AB 2 0.255771 0.453412 0.048139 21.00000 -1.50000
H8AC 2 0.312496 0.424905 0.089803 21.00000 -1.50000
AFIX 0
C9A 1 0.246998 0.482941 0.186796 21.00000 0.01670 0.03194 =
0.02753 0.00407 0.00365 -0.01299
AFIX 137
H9AA 2 0.257515 0.436285 0.203442 21.00000 -1.50000
H9AB 2 0.211905 0.481838 0.153611 21.00000 -1.50000
H9AC 2 0.244754 0.511461 0.232246 21.00000 -1.50000
AFIX 0
C6A 1 0.428906 0.471573 0.327374 21.00000 0.03376 0.02372 =
0.02375 0.00507 -0.00196 0.00536
AFIX 137
H6AA 2 0.457425 0.464938 0.295888 21.00000 -1.50000
H6AB 2 0.434608 0.440330 0.371707 21.00000 -1.50000
H6AC 2 0.429613 0.519007 0.345857 21.00000 -1.50000
AFIX 0
C2A 1 0.432576 0.486141 0.106648 21.00000 0.02006 0.01377 =
0.02013 -0.00160 0.00502 0.00011
AFIX 137
H2AA 2 0.447205 0.452388 0.145758 21.00000 -1.50000
H2AB 2 0.460687 0.500153 0.077003 21.00000 -1.50000
H2AC 2 0.402583 0.465754 0.071693 21.00000 -1.50000
AFIX 0
C1A 1 0.412680 0.548768 0.146431 21.00000 0.01526
AFIX 13
H1A 2 0.443453 0.567324 0.183640 21.00000 -1.20000
AFIX 0
C3A 1 0.395757 0.603654 0.084246 21.00000 0.01561
AFIX 137
H3AA 2 0.369854 0.583928 0.042496 21.00000 -1.50000
H3AB 2 0.427457 0.619626 0.063330 21.00000 -1.50000
H3AC 2 0.379189 0.642343 0.107332 21.00000 -1.50000
AFIX 0
PART 0
N1 3 0.362694 0.601045 0.256639 11.00000 0.03153 0.01424 =
0.02365 0.00861 -0.00034 -0.01171
PART -1
C1B 1 -0.085465 0.680310 0.262824 10.50000 0.09611
AFIX 137
H1BA 2 -0.110964 0.656035 0.224165 10.50000 -1.50000
H1BB 2 -0.089891 0.729837 0.255112 10.50000 -1.50000
H1BC 2 -0.092283 0.668189 0.314740 10.50000 -1.50000
AFIX 0
C1C 1 -0.026603 0.659277 0.253942 10.50000 0.08171
C1D 1 -0.012437 0.592555 0.250580 10.50000 0.06462
AFIX 43
H1D 2 -0.038157 0.557670 0.254543 10.50000 -1.20000
AFIX 0
C1E 1 0.039515 0.575007 0.241369 10.50000 0.09275
AFIX 43
H1E 2 0.048877 0.528118 0.237571 10.50000 -1.20000
AFIX 0
C1F 1 0.076752 0.623716 0.237763 10.50000 0.05762
AFIX 43
H1F 2 0.112151 0.610987 0.231203 10.50000 -1.20000
AFIX 0
C1G 1 0.063734 0.693227 0.243615 10.50000 0.08541
AFIX 43
H1G 2 0.090422 0.727672 0.244124 10.50000 -1.20000
AFIX 0
C1H 1 0.011239 0.710385 0.248616 10.50000 0.04485
AFIX 43
H1H 2 0.000887 0.757194 0.248425 10.50000 -1.20000
AFIX 0
HKLF 4
REM UBMGMZ in C2/c #15
REM R1 = 0.0331 for 7013 Fo > 4sig(Fo) and 0.0356 for all 7505 data
REM 499 parameters refined using 409 restraints
END
WGHT 0.0425 62.3729
REM Highest difference peak 2.108, deepest hole -2.193, 1-sigma level 0.146
Q1 1 0.4409 0.7114 0.2428 11.00000 0.05 2.11
Q2 1 0.3561 0.5422 0.2186 11.00000 0.05 2.08
Q3 1 0.0674 0.5981 0.2355 11.00000 0.05 1.88
Q4 1 0.0389 0.7264 0.2474 11.00000 0.05 1.83
Q5 1 0.3912 0.5130 0.2012 11.00000 0.05 1.77
Q6 1 0.3397 0.7119 0.2725 11.00000 0.05 1.69
Q7 1 -0.0177 0.6304 0.2564 11.00000 0.05 1.36
Q8 1 0.3825 0.6852 0.2137 11.00000 0.05 1.15
Q9 1 0.3941 0.6828 0.3006 11.00000 0.05 0.89
Q10 1 0.3466 0.6034 0.2520 11.00000 0.05 0.85
Q11 1 0.3928 0.7421 0.3059 11.00000 0.05 0.81
Q12 1 0.3767 0.7417 0.2020 11.00000 0.05 0.79
Q13 1 0.0000 0.6947 0.2500 10.50000 0.05 0.56
Q14 1 0.0899 0.6480 0.2395 11.00000 0.05 0.54
Q15 1 0.3900 0.7834 0.1835 11.00000 0.05 0.52
Q16 1 0.4572 0.7089 0.3366 11.00000 0.05 0.49
Q17 1 0.3848 0.7138 0.1554 11.00000 0.05 0.49
Q18 1 0.5179 0.6936 0.2026 11.00000 0.05 0.48
Q19 1 0.3942 0.6394 0.1808 11.00000 0.05 0.48
Q20 1 0.3955 0.7878 0.3287 11.00000 0.05 0.47
;
_shelx_res_checksum 10220
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
-16 0 0 0.0551 -16.0753 -0.0139 0.0007 -0.8448 -0.0034 -0.5235
16 0 0 0.0551 16.0753 0.0139 -0.0007 0.8448 0.0034 0.5235
-8 8 8 0.0846 -7.9753 7.9659 7.9772 -0.8085 0.2111 0.5799
8 -8 -8 0.1146 7.9753 -7.9659 -7.9772 0.8085 -0.2111 -0.5799
-7 -8 8 0.0788 -7.0348 -8.0092 7.9889 -0.4369 -0.8940 0.0952
7 8 -8 0.1038 7.0348 8.0092 -7.9889 0.4369 0.8940 -0.0952
7 -11 2 0.1033 6.9963 -10.9811 2.0035 0.5321 -0.8434 0.0191
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
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# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
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data_2
_database_code_depnum_ccdc_archive 'CCDC 1547173'
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_refine_special_details
;
'The C-C bond distances in the lattice THF molecule were restrained
to be approximately 1.55 A. Enhanced rigid bond restraints were applied to all atoms in the THF molecule.'
;
_vrf_PLAT972_2
;
PROBLEM: Check Calcd Residual Density 0.98A From U1 -3.81 eA-3
RESPONSE: Residual density is close to Uranium and
present despite applying adequate
absorption correction.
It is not chemically significant.
;
_audit_creation_date 2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C66 H150 N8 S Si6 U2, 2(C4 H8 O)'
_chemical_formula_sum 'C74 H166 N8 O2 S Si6 U2'
_chemical_formula_weight 1876.80
_chemical_melting_point ?
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'
S S 0.1246 0.1234 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 15
_space_group_name_H-M_alt 'C 1 2/c 1'
_space_group_name_Hall '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
_cell_length_a 29.155(6)
_cell_length_b 13.416(3)
_cell_length_c 22.949(5)
_cell_angle_alpha 90
_cell_angle_beta 105.344(4)
_cell_angle_gamma 90
_cell_volume 8657(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 2214
_cell_measurement_temperature 90(2)
_cell_measurement_theta_max 27.36
_cell_measurement_theta_min 2.63
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.889
_exptl_absorpt_correction_T_max 0.4305
_exptl_absorpt_correction_T_min 0.2792
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
'SADABS-2007/2 (Bruker,2007) was used for absorption correction. wR2(int) was 0.0923 before and 0.0632 after correction. The Ratio of minimum to maximum transmission is 0.6485. The \l/2 correction factor is 0.0015.'
_exptl_absorpt_special_details ?
_exptl_crystal_colour yellow
_exptl_crystal_colour_primary yellow
_exptl_crystal_density_diffrn 1.440
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description block
_exptl_crystal_F_000 3864
_exptl_crystal_preparation ?
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max 0.04
_exptl_crystal_size_mid 0.01
_exptl_crystal_size_min 0.01
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0908
_diffrn_reflns_av_unetI/netI 0.1205
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max 26
_diffrn_reflns_limit_h_min -34
_diffrn_reflns_limit_k_max 15
_diffrn_reflns_limit_k_min -15
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_limit_l_min -26
_diffrn_reflns_number 21439
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full 25.027
_diffrn_reflns_theta_max 25.027
_diffrn_reflns_theta_min 2.007
_diffrn_ambient_temperature 90(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source ?
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 5310
_reflns_number_total 7597
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2000)'
_computing_data_collection ?
_computing_data_reduction 'Bruker SAINT version 6.36A (Bruker, 2000)'
_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 'XS (Sheldrick, 2008)'
_refine_diff_density_max 1.511
_refine_diff_density_min -3.142
_refine_diff_density_rms 0.185
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.107
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 438
_refine_ls_number_reflns 7597
_refine_ls_number_restraints 33
_refine_ls_R_factor_all 0.1027
_refine_ls_R_factor_gt 0.0659
_refine_ls_restrained_S_all 1.109
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0264P)^2^+24.3120P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1056
_refine_ls_wR_factor_ref 0.1146
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
C37-C36 = C35-C34 = C36-C35
1.55 with sigma of 0.02
3. Rigid body (RIGU) restrains
O1, C34, C37, C35, C36
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4.a Ternary CH refined with riding coordinates:
C1(H1), C4(H4), C7(H7), C12(H12), C15(H15), C18(H18), C23(H23), C26(H26),
C29(H29)
4.b Secondary CH2 refined with riding coordinates:
C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
H32B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C36(H36A,H36B),
C37(H37A,H37B)
4.c Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C8(H8A,
H8B,H8C), C9(H9A,H9B,H9C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C16(H16A,
H16B,H16C), C17(H17A,H17B,H17C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
C24(H24A,H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,
H28C), C30(H30A,H30B,H30C), C31(H31A,H31B,H31C)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary difmap
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
U1 U 0.40596(2) 0.84830(3) 0.69675(2) 0.01241(10) Uani 1 1 d . . . . .
S1 S 0.500000 0.8480(3) 0.750000 0.0193(8) Uani 1 2 d S T P . .
Si1 Si 0.42229(10) 0.7712(2) 0.54936(13) 0.0151(6) Uani 1 1 d . . . . .
Si2 Si 0.39168(10) 1.1181(2) 0.71642(13) 0.0170(7) Uani 1 1 d . . . . .
Si3 Si 0.38085(10) 0.66874(19) 0.80598(13) 0.0162(6) Uani 1 1 d . . . . .
N1 N 0.3930(3) 0.7730(5) 0.6061(4) 0.0146(19) Uani 1 1 d . . . . .
N2 N 0.3766(3) 1.0046(6) 0.6798(3) 0.0126(18) Uani 1 1 d . . . . .
N3 N 0.3662(3) 0.7651(5) 0.7539(4) 0.0122(18) Uani 1 1 d . . . . .
N4 N 0.3119(3) 0.8440(7) 0.6409(3) 0.021(2) Uani 1 1 d . . . . .
C1 C 0.4496(3) 0.6435(8) 0.5419(4) 0.020(2) Uani 1 1 d . . . . .
H1 H 0.482070 0.645138 0.570711 0.024 Uiso 1 1 calc R . . . .
C2 C 0.4247(4) 0.5535(7) 0.5613(5) 0.025(3) Uani 1 1 d . . . . .
H2A H 0.420963 0.564966 0.601963 0.038 Uiso 1 1 calc GR . . . .
H2B H 0.443912 0.493495 0.561443 0.038 Uiso 1 1 calc GR . . . .
H2C H 0.393352 0.544583 0.532876 0.038 Uiso 1 1 calc GR . . . .
C3 C 0.4580(4) 0.6252(7) 0.4796(5) 0.025(3) Uani 1 1 d . . . . .
H3A H 0.427326 0.620617 0.449212 0.037 Uiso 1 1 calc GR . . . .
H3B H 0.475620 0.562817 0.480289 0.037 Uiso 1 1 calc GR . . . .
H3C H 0.476441 0.680564 0.469456 0.037 Uiso 1 1 calc GR . . . .
C4 C 0.4734(3) 0.8594(8) 0.5731(4) 0.018(2) Uani 1 1 d . . . . .
H4 H 0.495235 0.830985 0.610524 0.022 Uiso 1 1 calc R . . . .
C5 C 0.4599(3) 0.9661(7) 0.5895(5) 0.021(2) Uani 1 1 d . . . . .
H5A H 0.440363 0.998807 0.553268 0.032 Uiso 1 1 calc GR . . . .
H5B H 0.488983 1.004952 0.605693 0.032 Uiso 1 1 calc GR . . . .
H5C H 0.442009 0.961606 0.620047 0.032 Uiso 1 1 calc GR . . . .
C6 C 0.5024(3) 0.8697(7) 0.5269(4) 0.019(2) Uani 1 1 d . . . . .
H6A H 0.512914 0.803642 0.517588 0.029 Uiso 1 1 calc GR . . . .
H6B H 0.530184 0.911904 0.543628 0.029 Uiso 1 1 calc GR . . . .
H6C H 0.482651 0.900129 0.489909 0.029 Uiso 1 1 calc GR . . . .
C7 C 0.3842(4) 0.8054(7) 0.4714(5) 0.022(3) Uani 1 1 d . . . . .
H7 H 0.405962 0.797934 0.444515 0.026 Uiso 1 1 calc R . . . .
C8 C 0.3421(4) 0.7364(8) 0.4434(5) 0.031(3) Uani 1 1 d . . . . .
H8A H 0.352013 0.666835 0.451382 0.046 Uiso 1 1 calc GR . . . .
H8B H 0.331720 0.747564 0.399644 0.046 Uiso 1 1 calc GR . . . .
H8C H 0.315809 0.750824 0.461223 0.046 Uiso 1 1 calc GR . . . .
C9 C 0.3668(4) 0.9151(8) 0.4622(5) 0.028(3) Uani 1 1 d . . . . .
H9A H 0.348814 0.931398 0.491392 0.042 Uiso 1 1 calc GR . . . .
H9B H 0.346375 0.923440 0.421057 0.042 Uiso 1 1 calc GR . . . .
H9C H 0.394338 0.959586 0.468219 0.042 Uiso 1 1 calc GR . . . .
C10 C 0.3480(3) 0.7161(7) 0.5926(5) 0.016(2) Uani 1 1 d . . . . .
H10A H 0.348124 0.670214 0.626376 0.020 Uiso 1 1 calc R . . . .
H10B H 0.344865 0.675788 0.555575 0.020 Uiso 1 1 calc R . . . .
C11 C 0.3067(3) 0.7871(7) 0.5835(5) 0.019(2) Uani 1 1 d . . . . .
H11A H 0.306500 0.833532 0.549902 0.023 Uiso 1 1 calc R . . . .
H11B H 0.276320 0.749656 0.573320 0.023 Uiso 1 1 calc R . . . .
C12 C 0.4240(4) 1.2024(7) 0.6735(5) 0.022(3) Uani 1 1 d . . . . .
H12 H 0.456932 1.174425 0.681796 0.026 Uiso 1 1 calc R . . . .
C13 C 0.4054(4) 1.2011(8) 0.6056(5) 0.030(3) Uani 1 1 d . . . . .
H13A H 0.401439 1.131966 0.591380 0.045 Uiso 1 1 calc GR . . . .
H13B H 0.427977 1.235187 0.587485 0.045 Uiso 1 1 calc GR . . . .
H13C H 0.374615 1.235334 0.593810 0.045 Uiso 1 1 calc GR . . . .
C14 C 0.4308(5) 1.3105(8) 0.6945(5) 0.040(3) Uani 1 1 d . . . . .
H14A H 0.399812 1.340110 0.692970 0.059 Uiso 1 1 calc GR . . . .
H14B H 0.446002 1.347944 0.668007 0.059 Uiso 1 1 calc GR . . . .
H14C H 0.451042 1.312831 0.736060 0.059 Uiso 1 1 calc GR . . . .
C15 C 0.3393(4) 1.1905(7) 0.7304(5) 0.021(3) Uani 1 1 d . . . . .
H15 H 0.353620 1.251349 0.753150 0.025 Uiso 1 1 calc R . . . .
C16 C 0.3022(4) 1.2293(9) 0.6756(6) 0.042(3) Uani 1 1 d . . . . .
H16A H 0.317866 1.268348 0.650264 0.063 Uiso 1 1 calc GR . . . .
H16B H 0.279503 1.271686 0.688846 0.063 Uiso 1 1 calc GR . . . .
H16C H 0.285295 1.173051 0.652226 0.063 Uiso 1 1 calc GR . . . .
C17 C 0.3141(4) 1.1374(9) 0.7717(5) 0.034(3) Uani 1 1 d . . . . .
H17A H 0.302743 1.072258 0.754455 0.050 Uiso 1 1 calc GR . . . .
H17B H 0.286996 1.177600 0.775583 0.050 Uiso 1 1 calc GR . . . .
H17C H 0.336311 1.128176 0.811597 0.050 Uiso 1 1 calc GR . . . .
C18 C 0.4339(4) 1.0876(7) 0.7921(5) 0.020(3) Uani 1 1 d . . . . .
H18 H 0.464720 1.067603 0.784106 0.024 Uiso 1 1 calc R . . A 1
C19 C 0.4448(4) 1.1770(7) 0.8360(5) 0.029(3) Uani 1 1 d . . . B 1
H19A H 0.455914 1.233391 0.816262 0.043 Uiso 1 1 calc GR . . B 1
H19B H 0.469551 1.158208 0.872343 0.043 Uiso 1 1 calc GR . . B 1
H19C H 0.415886 1.196136 0.847343 0.043 Uiso 1 1 calc GR . . B 1
C20 C 0.4175(4) 0.9988(7) 0.8245(5) 0.026(3) Uani 1 1 d . . . . .
H20A H 0.382842 0.992337 0.810555 0.038 Uiso 1 1 calc GR . . . .
H20B H 0.426879 1.010306 0.868274 0.038 Uiso 1 1 calc GR . . . .
H20C H 0.432421 0.937357 0.815383 0.038 Uiso 1 1 calc GR . . . .
C21 C 0.3371(3) 1.0109(8) 0.6227(5) 0.019(2) Uani 1 1 d . . . . .
H21A H 0.326849 1.081100 0.614829 0.023 Uiso 1 1 calc R . . . .
H21B H 0.348460 0.986820 0.588187 0.023 Uiso 1 1 calc R . . . .
C22 C 0.2962(3) 0.9484(7) 0.6291(5) 0.023(3) Uani 1 1 d . . . . .
H22A H 0.284266 0.973748 0.662950 0.027 Uiso 1 1 calc R . . . .
H22B H 0.269908 0.952245 0.591640 0.027 Uiso 1 1 calc R . . . .
C23 C 0.3957(3) 0.7239(7) 0.8842(5) 0.018(2) Uani 1 1 d . . . . .
H23 H 0.422736 0.770614 0.885919 0.022 Uiso 1 1 calc R . . . .
C24 C 0.3557(4) 0.7893(8) 0.8966(5) 0.028(3) Uani 1 1 d . . . . .
H24A H 0.349234 0.845215 0.868183 0.042 Uiso 1 1 calc GR . . . .
H24B H 0.365664 0.814890 0.938076 0.042 Uiso 1 1 calc GR . . . .
H24C H 0.326799 0.749177 0.891546 0.042 Uiso 1 1 calc GR . . . .
C25 C 0.4137(3) 0.6521(8) 0.9385(4) 0.025(2) Uani 1 1 d . . . . .
H25A H 0.390205 0.599109 0.936764 0.038 Uiso 1 1 calc GR . . . .
H25B H 0.418126 0.689276 0.976384 0.038 Uiso 1 1 calc GR . . . .
H25C H 0.444011 0.622618 0.936727 0.038 Uiso 1 1 calc GR . . . .
C26 C 0.3283(4) 0.5781(7) 0.7940(5) 0.020(3) Uani 1 1 d . . . . .
H26 H 0.299588 0.621111 0.789953 0.024 Uiso 1 1 calc R . . . .
C27 C 0.3186(4) 0.5192(7) 0.7348(5) 0.021(3) Uani 1 1 d . . . . .
H27A H 0.318311 0.564969 0.701341 0.032 Uiso 1 1 calc GR . . . .
H27B H 0.287762 0.485766 0.727377 0.032 Uiso 1 1 calc GR . . . .
H27C H 0.343709 0.469374 0.737653 0.032 Uiso 1 1 calc GR . . . .
C28 C 0.3282(4) 0.5061(8) 0.8457(5) 0.032(3) Uani 1 1 d . . . . .
H28A H 0.357585 0.466797 0.855294 0.048 Uiso 1 1 calc GR . . . .
H28B H 0.300766 0.461361 0.833534 0.048 Uiso 1 1 calc GR . . . .
H28C H 0.326247 0.544111 0.881445 0.048 Uiso 1 1 calc GR . . . .
C29 C 0.4355(3) 0.6048(7) 0.7939(5) 0.015(2) Uani 1 1 d . . . . .
H29 H 0.463083 0.649759 0.811167 0.018 Uiso 1 1 calc R . . . .
C30 C 0.4339(4) 0.5890(7) 0.7267(4) 0.020(2) Uani 1 1 d . . . . .
H30A H 0.404898 0.552436 0.706649 0.030 Uiso 1 1 calc GR . . . .
H30B H 0.461789 0.550592 0.723856 0.030 Uiso 1 1 calc GR . . . .
H30C H 0.433912 0.653822 0.707116 0.030 Uiso 1 1 calc GR . . . .
C31 C 0.4473(3) 0.5025(7) 0.8266(5) 0.021(3) Uani 1 1 d . . . . .
H31A H 0.448524 0.510384 0.869428 0.032 Uiso 1 1 calc GR . . . .
H31B H 0.478184 0.478877 0.822803 0.032 Uiso 1 1 calc GR . . . .
H31C H 0.422615 0.453971 0.808109 0.032 Uiso 1 1 calc GR . . . .
C32 C 0.3177(3) 0.8103(7) 0.7464(5) 0.018(2) Uani 1 1 d . . . . .
H32A H 0.320848 0.882607 0.755268 0.022 Uiso 1 1 calc R . . . .
H32B H 0.302011 0.779019 0.775132 0.022 Uiso 1 1 calc R . . . .
C33 C 0.2879(3) 0.7942(7) 0.6825(5) 0.019(2) Uani 1 1 d . . . . .
H33A H 0.284647 0.721994 0.673462 0.023 Uiso 1 1 calc R . . . .
H33B H 0.255786 0.822616 0.677382 0.023 Uiso 1 1 calc R . . . .
O1 O 0.2462(4) 1.1147(7) 0.5205(5) 0.065(3) Uani 1 1 d . U . . .
C34 C 0.2010(6) 1.0909(15) 0.4941(7) 0.091(6) Uani 1 1 d D U . . .
H34A H 0.181092 1.151778 0.487702 0.109 Uiso 1 1 calc R . . . .
H34B H 0.188901 1.045187 0.520539 0.109 Uiso 1 1 calc R . . . .
C35 C 0.1979(5) 1.0418(13) 0.4351(8) 0.087(6) Uani 1 1 d D U . . .
H35A H 0.177053 1.079946 0.401454 0.104 Uiso 1 1 calc R . . . .
H35B H 0.185548 0.973010 0.434566 0.104 Uiso 1 1 calc R . . . .
C36 C 0.2491(4) 1.0416(11) 0.4305(6) 0.062(4) Uani 1 1 d D U . . .
H36A H 0.264609 0.976371 0.442384 0.075 Uiso 1 1 calc R . . . .
H36B H 0.250874 1.058642 0.389174 0.075 Uiso 1 1 calc R . . . .
C37 C 0.2704(5) 1.1216(10) 0.4749(6) 0.052(4) Uani 1 1 d D U . . .
H37A H 0.304912 1.110359 0.491838 0.062 Uiso 1 1 calc R . . . .
H37B H 0.265549 1.188010 0.455433 0.062 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
U1 0.01333(18) 0.01365(17) 0.01091(18) 0.0005(2) 0.00439(12) 0.0009(2)
S1 0.0161(19) 0.0199(19) 0.021(2) 0.000 0.0029(16) 0.000
Si1 0.0161(15) 0.0195(15) 0.0113(16) 0.0006(12) 0.0065(12) 0.0005(12)
Si2 0.0194(16) 0.0156(15) 0.0157(17) 0.0008(12) 0.0043(12) 0.0043(11)
Si3 0.0196(15) 0.0126(16) 0.0172(16) 0.0032(12) 0.0063(12) 0.0000(12)
N1 0.011(4) 0.010(4) 0.024(5) 0.001(4) 0.007(4) 0.001(3)
N2 0.012(4) 0.020(5) 0.004(5) -0.001(3) -0.001(3) 0.008(3)
N3 0.012(4) 0.015(4) 0.013(5) 0.007(4) 0.009(4) 0.007(3)
N4 0.022(5) 0.025(5) 0.016(5) 0.003(4) 0.007(4) 0.000(4)
C1 0.023(6) 0.020(5) 0.019(6) -0.010(5) 0.007(4) 0.002(5)
C2 0.039(7) 0.018(6) 0.022(7) -0.009(5) 0.014(6) -0.002(5)
C3 0.025(6) 0.020(6) 0.028(7) 0.002(5) 0.006(5) 0.007(5)
C4 0.021(5) 0.027(6) 0.012(5) -0.005(5) 0.013(4) -0.001(5)
C5 0.025(6) 0.024(6) 0.014(6) -0.005(5) 0.005(5) 0.000(5)
C6 0.020(6) 0.027(7) 0.013(6) -0.005(5) 0.009(4) -0.006(5)
C7 0.025(6) 0.023(6) 0.014(6) 0.000(5) -0.001(5) -0.005(5)
C8 0.024(7) 0.048(8) 0.021(7) 0.001(6) 0.007(5) 0.006(6)
C9 0.023(6) 0.025(6) 0.035(8) 0.006(5) 0.006(5) 0.011(5)
C10 0.018(6) 0.020(6) 0.010(6) -0.005(4) 0.001(4) -0.006(4)
C11 0.019(6) 0.027(6) 0.010(6) -0.006(5) -0.001(4) -0.003(5)
C12 0.020(6) 0.009(5) 0.035(7) 0.006(5) 0.006(5) 0.001(4)
C13 0.051(8) 0.017(6) 0.028(8) -0.005(5) 0.020(6) -0.003(5)
C14 0.066(9) 0.032(7) 0.021(7) 0.000(5) 0.013(7) -0.011(6)
C15 0.026(6) 0.022(6) 0.017(6) -0.005(5) 0.012(5) 0.000(5)
C16 0.038(8) 0.049(8) 0.036(9) -0.007(7) 0.004(6) 0.022(6)
C17 0.018(6) 0.060(9) 0.026(7) -0.005(7) 0.012(5) 0.007(6)
C18 0.018(6) 0.024(6) 0.020(7) 0.001(5) 0.009(5) 0.003(5)
C19 0.032(7) 0.030(7) 0.018(7) 0.002(5) -0.002(5) -0.003(5)
C20 0.021(6) 0.024(6) 0.028(7) 0.000(5) 0.000(5) 0.003(5)
C21 0.015(6) 0.029(6) 0.018(6) 0.002(5) 0.011(5) 0.005(5)
C22 0.021(6) 0.024(6) 0.020(6) 0.002(5) 0.001(5) 0.003(5)
C23 0.018(6) 0.022(6) 0.017(6) 0.003(5) 0.009(5) -0.004(4)
C24 0.034(7) 0.037(7) 0.011(6) -0.008(5) 0.003(5) 0.006(5)
C25 0.034(6) 0.024(6) 0.017(6) 0.000(6) 0.006(5) 0.002(6)
C26 0.027(6) 0.017(6) 0.017(6) 0.007(5) 0.007(5) -0.003(5)
C27 0.021(6) 0.019(6) 0.026(7) -0.003(5) 0.009(5) -0.007(5)
C28 0.035(7) 0.030(7) 0.033(8) 0.011(6) 0.012(6) -0.008(5)
C29 0.007(5) 0.019(5) 0.017(6) 0.002(4) 0.001(4) -0.002(4)
C30 0.025(6) 0.019(6) 0.017(6) 0.011(4) 0.008(5) 0.014(5)
C31 0.013(6) 0.032(6) 0.022(7) 0.011(5) 0.012(5) 0.006(5)
C32 0.023(6) 0.020(5) 0.016(6) 0.012(4) 0.013(5) 0.005(4)
C33 0.018(6) 0.019(6) 0.021(6) 0.004(5) 0.007(5) 0.006(4)
O1 0.071(6) 0.086(8) 0.044(6) 0.001(5) 0.024(5) 0.007(6)
C34 0.050(7) 0.170(19) 0.059(11) 0.008(10) 0.023(7) 0.019(9)
C35 0.064(8) 0.092(13) 0.113(13) -0.041(11) 0.038(9) -0.045(9)
C36 0.044(7) 0.091(11) 0.044(9) -0.012(7) -0.002(6) 0.038(7)
C37 0.043(7) 0.075(10) 0.041(8) 0.016(6) 0.016(6) -0.010(6)
_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
U1 S1 2.6903(6) . ?
U1 N1 2.253(8) . ?
U1 N2 2.259(7) . ?
U1 N3 2.261(8) . ?
U1 N4 2.704(7) . ?
Si1 N1 1.735(8) . ?
Si1 C1 1.917(10) . ?
Si1 C4 1.867(10) . ?
Si1 C7 1.896(10) . ?
Si2 N2 1.740(8) . ?
Si2 C12 1.906(10) . ?
Si2 C15 1.907(10) . ?
Si2 C18 1.889(11) . ?
Si3 N3 1.735(8) . ?
Si3 C23 1.884(10) . ?
Si3 C26 1.919(10) . ?
Si3 C29 1.894(10) . ?
N1 C10 1.479(11) . ?
N2 C21 1.499(12) . ?
N3 C32 1.507(11) . ?
N4 C11 1.494(12) . ?
N4 C22 1.476(13) . ?
N4 C33 1.482(12) . ?
C1 H1 1.0000 . ?
C1 C2 1.534(14) . ?
C1 C3 1.533(13) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4 1.0000 . ?
C4 C5 1.556(13) . ?
C4 C6 1.527(12) . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7 1.0000 . ?
C7 C8 1.535(13) . ?
C7 C9 1.552(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C10 C11 1.508(13) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 H12 1.0000 . ?
C12 C13 1.508(14) . ?
C12 C14 1.524(13) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 1.0000 . ?
C15 C16 1.517(14) . ?
C15 C17 1.521(14) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.545(14) . ?
C18 C20 1.547(14) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C22 1.499(13) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 H23 1.0000 . ?
C23 C24 1.545(13) . ?
C23 C25 1.552(13) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26 1.0000 . ?
C26 C27 1.532(14) . ?
C26 C28 1.531(13) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29 1.0000 . ?
C29 C30 1.543(13) . ?
C29 C31 1.558(13) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C33 1.509(13) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O1 C34 1.336(17) . ?
O1 C37 1.411(15) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C34 C35 1.487(15) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.522(13) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36 C37 1.498(13) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
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
S1 U1 N4 178.18(19) . . ?
N1 U1 S1 108.66(19) . . ?
N1 U1 N2 107.1(3) . . ?
N1 U1 N3 109.2(3) . . ?
N1 U1 N4 69.6(3) . . ?
N2 U1 S1 112.0(2) . . ?
N2 U1 N3 109.2(3) . . ?
N2 U1 N4 69.3(3) . . ?
N3 U1 S1 110.65(19) . . ?
N3 U1 N4 69.7(3) . . ?
U1 S1 U1 179.81(18) 2_656 . ?
N1 Si1 C1 112.2(4) . . ?
N1 Si1 C4 106.6(4) . . ?
N1 Si1 C7 115.0(5) . . ?
C4 Si1 C1 105.9(4) . . ?
C4 Si1 C7 110.2(5) . . ?
C7 Si1 C1 106.6(5) . . ?
N2 Si2 C12 111.5(4) . . ?
N2 Si2 C15 114.5(4) . . ?
N2 Si2 C18 105.9(4) . . ?
C12 Si2 C15 108.2(4) . . ?
C18 Si2 C12 108.2(5) . . ?
C18 Si2 C15 108.2(5) . . ?
N3 Si3 C23 108.5(4) . . ?
N3 Si3 C26 109.4(4) . . ?
N3 Si3 C29 107.4(4) . . ?
C23 Si3 C26 111.0(5) . . ?
C23 Si3 C29 109.1(4) . . ?
C29 Si3 C26 111.3(5) . . ?
Si1 N1 U1 134.7(4) . . ?
C10 N1 U1 110.3(6) . . ?
C10 N1 Si1 114.9(6) . . ?
Si2 N2 U1 133.9(4) . . ?
C21 N2 U1 111.8(6) . . ?
C21 N2 Si2 114.2(6) . . ?
Si3 N3 U1 134.2(4) . . ?
C32 N3 U1 110.1(5) . . ?
C32 N3 Si3 115.5(6) . . ?
C11 N4 U1 106.4(5) . . ?
C22 N4 U1 107.0(6) . . ?
C22 N4 C11 111.7(8) . . ?
C22 N4 C33 111.7(8) . . ?
C33 N4 U1 107.2(6) . . ?
C33 N4 C11 112.5(8) . . ?
Si1 C1 H1 105.3 . . ?
C2 C1 Si1 115.9(7) . . ?
C2 C1 H1 105.3 . . ?
C3 C1 Si1 113.5(7) . . ?
C3 C1 H1 105.3 . . ?
C3 C1 C2 110.5(8) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
Si1 C4 H4 106.7 . . ?
C5 C4 Si1 114.9(7) . . ?
C5 C4 H4 106.7 . . ?
C6 C4 Si1 113.6(7) . . ?
C6 C4 H4 106.7 . . ?
C6 C4 C5 107.9(8) . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
Si1 C7 H7 104.4 . . ?
C8 C7 Si1 116.9(7) . . ?
C8 C7 H7 104.4 . . ?
C8 C7 C9 108.6(9) . . ?
C9 C7 Si1 116.5(7) . . ?
C9 C7 H7 104.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 H10A 109.7 . . ?
N1 C10 H10B 109.7 . . ?
N1 C10 C11 109.6(8) . . ?
H10A C10 H10B 108.2 . . ?
C11 C10 H10A 109.7 . . ?
C11 C10 H10B 109.7 . . ?
N4 C11 C10 108.1(8) . . ?
N4 C11 H11A 110.1 . . ?
N4 C11 H11B 110.1 . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
Si2 C12 H12 105.0 . . ?
C13 C12 Si2 115.8(7) . . ?
C13 C12 H12 105.0 . . ?
C13 C12 C14 108.6(8) . . ?
C14 C12 Si2 116.1(8) . . ?
C14 C12 H12 105.0 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
Si2 C15 H15 105.1 . . ?
C16 C15 Si2 117.6(8) . . ?
C16 C15 H15 105.1 . . ?
C16 C15 C17 108.8(9) . . ?
C17 C15 Si2 114.0(7) . . ?
C17 C15 H15 105.1 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
Si2 C18 H18 106.8 . . ?
C19 C18 Si2 113.8(7) . . ?
C19 C18 H18 106.8 . . ?
C19 C18 C20 108.7(9) . . ?
C20 C18 Si2 113.6(7) . . ?
C20 C18 H18 106.8 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 H21A 109.8 . . ?
N2 C21 H21B 109.8 . . ?
H21A C21 H21B 108.3 . . ?
C22 C21 N2 109.2(8) . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
N4 C22 C21 109.4(8) . . ?
N4 C22 H22A 109.8 . . ?
N4 C22 H22B 109.8 . . ?
C21 C22 H22A 109.8 . . ?
C21 C22 H22B 109.8 . . ?
H22A C22 H22B 108.2 . . ?
Si3 C23 H23 105.2 . . ?
C24 C23 Si3 113.9(7) . . ?
C24 C23 H23 105.2 . . ?
C24 C23 C25 108.4(8) . . ?
C25 C23 Si3 117.7(7) . . ?
C25 C23 H23 105.2 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si3 C26 H26 105.3 . . ?
C27 C26 Si3 113.9(7) . . ?
C27 C26 H26 105.3 . . ?
C28 C26 Si3 116.9(7) . . ?
C28 C26 H26 105.3 . . ?
C28 C26 C27 109.0(8) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
Si3 C29 H29 106.7 . . ?
C30 C29 Si3 113.8(7) . . ?
C30 C29 H29 106.7 . . ?
C30 C29 C31 107.7(8) . . ?
C31 C29 Si3 114.6(7) . . ?
C31 C29 H29 106.7 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 H32A 109.8 . . ?
N3 C32 H32B 109.8 . . ?
N3 C32 C33 109.5(8) . . ?
H32A C32 H32B 108.2 . . ?
C33 C32 H32A 109.8 . . ?
C33 C32 H32B 109.8 . . ?
N4 C33 C32 108.3(8) . . ?
N4 C33 H33A 110.0 . . ?
N4 C33 H33B 110.0 . . ?
C32 C33 H33A 110.0 . . ?
C32 C33 H33B 110.0 . . ?
H33A C33 H33B 108.4 . . ?
C34 O1 C37 107.9(12) . . ?
O1 C34 H34A 109.8 . . ?
O1 C34 H34B 109.8 . . ?
O1 C34 C35 109.4(13) . . ?
H34A C34 H34B 108.2 . . ?
C35 C34 H34A 109.8 . . ?
C35 C34 H34B 109.8 . . ?
C34 C35 H35A 111.0 . . ?
C34 C35 H35B 111.0 . . ?
C34 C35 C36 104.0(12) . . ?
H35A C35 H35B 109.0 . . ?
C36 C35 H35A 111.0 . . ?
C36 C35 H35B 111.0 . . ?
C35 C36 H36A 111.6 . . ?
C35 C36 H36B 111.6 . . ?
H36A C36 H36B 109.4 . . ?
C37 C36 C35 100.9(10) . . ?
C37 C36 H36A 111.6 . . ?
C37 C36 H36B 111.6 . . ?
O1 C37 C36 105.0(10) . . ?
O1 C37 H37A 110.7 . . ?
O1 C37 H37B 110.7 . . ?
C36 C37 H37A 110.7 . . ?
C36 C37 H37B 110.7 . . ?
H37A C37 H37B 108.8 . . ?
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
U1 N1 C10 C11 67.3(8) . . . . ?
U1 N2 C21 C22 64.1(9) . . . . ?
U1 N3 C32 C33 66.2(8) . . . . ?
U1 N4 C11 C10 26.8(9) . . . . ?
U1 N4 C22 C21 27.8(9) . . . . ?
U1 N4 C33 C32 27.2(9) . . . . ?
Si1 N1 C10 C11 -110.4(8) . . . . ?
Si2 N2 C21 C22 -118.7(8) . . . . ?
Si3 N3 C32 C33 -117.4(7) . . . . ?
N1 Si1 C4 C5 -53.3(8) . . . . ?
N1 Si1 C4 C6 -178.1(7) . . . . ?
N1 Si1 C7 C8 -63.0(9) . . . . ?
N1 Si1 C7 C9 67.7(9) . . . . ?
N1 C10 C11 N4 -61.3(10) . . . . ?
N2 Si2 C18 C19 -170.1(7) . . . . ?
N2 Si2 C18 C20 -45.0(8) . . . . ?
N2 C21 C22 N4 -59.5(10) . . . . ?
N3 Si3 C23 C24 56.1(8) . . . . ?
N3 Si3 C23 C25 -175.5(7) . . . . ?
N3 Si3 C29 C30 -42.5(8) . . . . ?
N3 Si3 C29 C31 -167.1(7) . . . . ?
N3 C32 C33 N4 -60.8(10) . . . . ?
C1 Si1 N1 U1 111.9(6) . . . . ?
C1 Si1 N1 C10 -71.1(7) . . . . ?
C1 Si1 C4 C5 -172.9(7) . . . . ?
C1 Si1 C4 C6 62.2(8) . . . . ?
C1 Si1 C7 C8 62.0(9) . . . . ?
C1 Si1 C7 C9 -167.2(8) . . . . ?
C4 Si1 N1 U1 -3.6(7) . . . . ?
C4 Si1 N1 C10 173.4(6) . . . . ?
C4 Si1 C7 C8 176.5(8) . . . . ?
C4 Si1 C7 C9 -52.7(9) . . . . ?
C7 Si1 N1 U1 -126.0(6) . . . . ?
C7 Si1 N1 C10 51.0(7) . . . . ?
C7 Si1 C4 C5 72.2(8) . . . . ?
C7 Si1 C4 C6 -52.7(9) . . . . ?
C11 N4 C22 C21 -88.3(10) . . . . ?
C11 N4 C33 C32 143.8(8) . . . . ?
C12 Si2 N2 U1 104.6(6) . . . . ?
C12 Si2 N2 C21 -71.8(7) . . . . ?
C12 Si2 C18 C19 70.3(8) . . . . ?
C12 Si2 C18 C20 -164.7(7) . . . . ?
C15 Si2 N2 U1 -132.1(6) . . . . ?
C15 Si2 N2 C21 51.5(8) . . . . ?
C15 Si2 C18 C19 -46.8(9) . . . . ?
C15 Si2 C18 C20 78.3(8) . . . . ?
C18 Si2 N2 U1 -12.9(7) . . . . ?
C18 Si2 N2 C21 170.7(7) . . . . ?
C22 N4 C11 C10 143.3(8) . . . . ?
C22 N4 C33 C32 -89.7(9) . . . . ?
C23 Si3 N3 U1 99.7(6) . . . . ?
C23 Si3 N3 C32 -75.5(7) . . . . ?
C23 Si3 C29 C30 -159.9(7) . . . . ?
C23 Si3 C29 C31 75.5(8) . . . . ?
C26 Si3 N3 U1 -139.0(6) . . . . ?
C26 Si3 N3 C32 45.7(8) . . . . ?
C26 Si3 C23 C24 -64.1(8) . . . . ?
C26 Si3 C23 C25 64.3(8) . . . . ?
C26 Si3 C29 C30 77.2(8) . . . . ?
C26 Si3 C29 C31 -47.4(9) . . . . ?
C29 Si3 N3 U1 -18.1(7) . . . . ?
C29 Si3 N3 C32 166.6(7) . . . . ?
C29 Si3 C23 C24 172.8(7) . . . . ?
C29 Si3 C23 C25 -58.7(8) . . . . ?
C33 N4 C11 C10 -90.2(9) . . . . ?
C33 N4 C22 C21 144.8(9) . . . . ?
O1 C34 C35 C36 -1(2) . . . . ?
C34 O1 C37 C36 -36.3(15) . . . . ?
C34 C35 C36 C37 -19.8(18) . . . . ?
C35 C36 C37 O1 33.5(15) . . . . ?
C37 O1 C34 C35 22.9(19) . . . . ?
_shelx_res_file
;
TITL UDKING in C2/c #15
udking.res
created by SHELXL-2016/6 at 14:45:02 on 27-Apr-2017
REM reset to C2/c #15
REM EXTI insignif
CELL 0.71073 29.1551 13.4163 22.949 90 105.344 90
ZERR 4 0.0056 0.0027 0.0046 0 0.004 0
LATT 7
SYMM -X,+Y,0.5-Z
SFAC C H N O S Si U
UNIT 296 664 32 8 4 24 8
DFIX 1.55 C37 C36 C35 C34 C36 C35
RIGU O1 C34 C37 C35 C36
L.S. 64
PLAN 20
TEMP -183(2)
BOND $H
CONF
HTAB
MORE -1
fmap 2
acta
SHEL 100 0.84
OMIT 29 7 0
OMIT 28 8 1
OMIT 24 10 1
OMIT 26 8 2
REM
REM
REM
WGHT 0.026400 24.312000
FVAR 0.03662
U1 7 0.405958 0.848296 0.696755 11.00000 0.01333 0.01365 =
0.01091 0.00050 0.00439 0.00088
S1 5 0.500000 0.847957 0.750000 10.50000 0.01612 0.01986 =
0.02078 0.00000 0.00293 0.00000
SI1 6 0.422293 0.771239 0.549357 11.00000 0.01610 0.01948 =
0.01131 0.00060 0.00647 0.00045
SI2 6 0.391677 1.118136 0.716424 11.00000 0.01942 0.01562 =
0.01568 0.00078 0.00426 0.00434
SI3 6 0.380848 0.668745 0.805977 11.00000 0.01963 0.01259 =
0.01718 0.00317 0.00633 0.00004
N1 3 0.393033 0.773017 0.606088 11.00000 0.01070 0.01035 =
0.02392 0.00123 0.00683 0.00075
N2 3 0.376574 1.004560 0.679764 11.00000 0.01176 0.02005 =
0.00422 -0.00081 -0.00115 0.00841
N3 3 0.366219 0.765079 0.753918 11.00000 0.01194 0.01494 =
0.01285 0.00670 0.00880 0.00662
N4 3 0.311868 0.844008 0.640866 11.00000 0.02244 0.02508 =
0.01615 0.00263 0.00727 -0.00023
C1 1 0.449645 0.643458 0.541929 11.00000 0.02284 0.01981 =
0.01897 -0.00972 0.00658 0.00174
AFIX 13
H1 2 0.482070 0.645138 0.570711 11.00000 -1.20000
AFIX 0
C2 1 0.424717 0.553503 0.561302 11.00000 0.03946 0.01786 =
0.02227 -0.00911 0.01379 -0.00239
AFIX 137
H2A 2 0.420963 0.564966 0.601963 11.00000 -1.50000
H2B 2 0.443912 0.493495 0.561443 11.00000 -1.50000
H2C 2 0.393352 0.544583 0.532876 11.00000 -1.50000
AFIX 0
C3 1 0.458013 0.625220 0.479600 11.00000 0.02454 0.02044 =
0.02807 0.00243 0.00566 0.00662
AFIX 137
H3A 2 0.427326 0.620617 0.449212 11.00000 -1.50000
H3B 2 0.475620 0.562817 0.480289 11.00000 -1.50000
H3C 2 0.476441 0.680564 0.469456 11.00000 -1.50000
AFIX 0
C4 1 0.473378 0.859433 0.573091 11.00000 0.02111 0.02719 =
0.01180 -0.00466 0.01303 -0.00056
AFIX 13
H4 2 0.495235 0.830985 0.610524 11.00000 -1.20000
AFIX 0
C5 1 0.459940 0.966068 0.589548 11.00000 0.02474 0.02434 =
0.01430 -0.00462 0.00531 -0.00044
AFIX 137
H5A 2 0.440363 0.998807 0.553268 11.00000 -1.50000
H5B 2 0.488983 1.004952 0.605693 11.00000 -1.50000
H5C 2 0.442009 0.961606 0.620047 11.00000 -1.50000
AFIX 0
C6 1 0.502378 0.869696 0.526921 11.00000 0.02048 0.02695 =
0.01325 -0.00511 0.00873 -0.00591
AFIX 137
H6A 2 0.512914 0.803642 0.517588 11.00000 -1.50000
H6B 2 0.530184 0.911904 0.543628 11.00000 -1.50000
H6C 2 0.482651 0.900129 0.489909 11.00000 -1.50000
AFIX 0
C7 1 0.384189 0.805416 0.471373 11.00000 0.02467 0.02306 =
0.01356 -0.00005 -0.00131 -0.00462
AFIX 13
H7 2 0.405962 0.797934 0.444515 11.00000 -1.20000
AFIX 0
C8 1 0.342131 0.736423 0.443375 11.00000 0.02415 0.04763 =
0.02086 0.00107 0.00666 0.00578
AFIX 137
H8A 2 0.352013 0.666835 0.451382 11.00000 -1.50000
H8B 2 0.331720 0.747564 0.399644 11.00000 -1.50000
H8C 2 0.315809 0.750824 0.461223 11.00000 -1.50000
AFIX 0
C9 1 0.366830 0.915061 0.462162 11.00000 0.02307 0.02474 =
0.03538 0.00605 0.00614 0.01108
AFIX 137
H9A 2 0.348814 0.931398 0.491392 11.00000 -1.50000
H9B 2 0.346375 0.923440 0.421057 11.00000 -1.50000
H9C 2 0.394338 0.959586 0.468219 11.00000 -1.50000
AFIX 0
C10 1 0.348011 0.716106 0.592557 11.00000 0.01786 0.01966 =
0.01028 -0.00471 0.00121 -0.00577
AFIX 23
H10A 2 0.348124 0.670214 0.626376 11.00000 -1.20000
H10B 2 0.344865 0.675788 0.555575 11.00000 -1.20000
AFIX 0
C11 1 0.306652 0.787132 0.583496 11.00000 0.01904 0.02660 =
0.00982 -0.00592 -0.00084 -0.00288
AFIX 23
H11A 2 0.306500 0.833532 0.549902 11.00000 -1.20000
H11B 2 0.276320 0.749656 0.573320 11.00000 -1.20000
AFIX 0
C12 1 0.424043 1.202419 0.673453 11.00000 0.02038 0.00943 =
0.03532 0.00575 0.00571 0.00143
AFIX 13
H12 2 0.456932 1.174425 0.681796 11.00000 -1.20000
AFIX 0
C13 1 0.405386 1.201112 0.605594 11.00000 0.05128 0.01658 =
0.02797 -0.00476 0.02009 -0.00347
AFIX 137
H13A 2 0.401439 1.131966 0.591380 11.00000 -1.50000
H13B 2 0.427977 1.235187 0.587485 11.00000 -1.50000
H13C 2 0.374615 1.235334 0.593810 11.00000 -1.50000
AFIX 0
C14 1 0.430831 1.310472 0.694501 11.00000 0.06570 0.03241 =
0.02137 -0.00039 0.01297 -0.01075
AFIX 137
H14A 2 0.399812 1.340110 0.692970 11.00000 -1.50000
H14B 2 0.446002 1.347944 0.668007 11.00000 -1.50000
H14C 2 0.451042 1.312831 0.736060 11.00000 -1.50000
AFIX 0
C15 1 0.339270 1.190466 0.730359 11.00000 0.02636 0.02214 =
0.01669 -0.00518 0.01173 0.00002
AFIX 13
H15 2 0.353620 1.251349 0.753150 11.00000 -1.20000
AFIX 0
C16 1 0.302203 1.229327 0.675575 11.00000 0.03814 0.04898 =
0.03559 -0.00697 0.00354 0.02184
AFIX 137
H16A 2 0.317866 1.268348 0.650264 11.00000 -1.50000
H16B 2 0.279503 1.271686 0.688846 11.00000 -1.50000
H16C 2 0.285295 1.173051 0.652226 11.00000 -1.50000
AFIX 0
C17 1 0.314092 1.137408 0.771671 11.00000 0.01837 0.05975 =
0.02601 -0.00541 0.01157 0.00669
AFIX 137
H17A 2 0.302743 1.072258 0.754455 11.00000 -1.50000
H17B 2 0.286996 1.177600 0.775583 11.00000 -1.50000
H17C 2 0.336311 1.128176 0.811597 11.00000 -1.50000
AFIX 0
C18 1 0.433905 1.087620 0.792092 11.00000 0.01755 0.02383 =
0.02047 0.00101 0.00920 0.00284
PART 1
AFIX 13
H18 2 0.464720 1.067603 0.784106 11.00000 -1.20000
AFIX 0
C19 1 0.444811 1.177009 0.836026 11.00000 0.03241 0.03038 =
0.01795 0.00200 -0.00182 -0.00288
AFIX 137
H19A 2 0.455914 1.233391 0.816262 11.00000 -1.50000
H19B 2 0.469551 1.158208 0.872343 11.00000 -1.50000
H19C 2 0.415886 1.196136 0.847343 11.00000 -1.50000
AFIX 0
PART 0
C20 1 0.417510 0.998764 0.824550 11.00000 0.02054 0.02388 =
0.02847 -0.00035 0.00009 0.00348
AFIX 137
H20A 2 0.382842 0.992337 0.810555 11.00000 -1.50000
H20B 2 0.426879 1.010306 0.868274 11.00000 -1.50000
H20C 2 0.432421 0.937357 0.815383 11.00000 -1.50000
AFIX 0
C21 1 0.337135 1.010936 0.622717 11.00000 0.01497 0.02856 =
0.01844 0.00233 0.01147 0.00457
AFIX 23
H21A 2 0.326849 1.081100 0.614829 11.00000 -1.20000
H21B 2 0.348460 0.986820 0.588187 11.00000 -1.20000
AFIX 0
C22 1 0.296155 0.948432 0.629134 11.00000 0.02112 0.02422 =
0.01976 0.00170 0.00105 0.00343
AFIX 23
H22A 2 0.284266 0.973748 0.662950 11.00000 -1.20000
H22B 2 0.269908 0.952245 0.591640 11.00000 -1.20000
AFIX 0
C23 1 0.395695 0.723884 0.884239 11.00000 0.01795 0.02199 =
0.01698 0.00254 0.00942 -0.00389
AFIX 13
H23 2 0.422736 0.770614 0.885919 11.00000 -1.20000
AFIX 0
C24 1 0.355691 0.789268 0.896645 11.00000 0.03443 0.03660 =
0.01100 -0.00789 0.00264 0.00590
AFIX 137
H24A 2 0.349234 0.845215 0.868183 11.00000 -1.50000
H24B 2 0.365664 0.814890 0.938076 11.00000 -1.50000
H24C 2 0.326799 0.749177 0.891546 11.00000 -1.50000
AFIX 0
C25 1 0.413665 0.652108 0.938531 11.00000 0.03385 0.02425 =
0.01709 0.00034 0.00594 0.00214
AFIX 137
H25A 2 0.390205 0.599109 0.936764 11.00000 -1.50000
H25B 2 0.418126 0.689276 0.976384 11.00000 -1.50000
H25C 2 0.444011 0.622618 0.936727 11.00000 -1.50000
AFIX 0
C26 1 0.328256 0.578054 0.793971 11.00000 0.02670 0.01735 =
0.01683 0.00650 0.00710 -0.00257
AFIX 13
H26 2 0.299588 0.621111 0.789953 11.00000 -1.20000
AFIX 0
C27 1 0.318644 0.519245 0.734752 11.00000 0.02086 0.01872 =
0.02608 -0.00309 0.00850 -0.00656
AFIX 137
H27A 2 0.318311 0.564969 0.701341 11.00000 -1.50000
H27B 2 0.287762 0.485766 0.727377 11.00000 -1.50000
H27C 2 0.343709 0.469374 0.737653 11.00000 -1.50000
AFIX 0
C28 1 0.328209 0.506111 0.845714 11.00000 0.03516 0.03009 =
0.03345 0.01137 0.01232 -0.00804
AFIX 137
H28A 2 0.357585 0.466797 0.855294 11.00000 -1.50000
H28B 2 0.300766 0.461361 0.833534 11.00000 -1.50000
H28C 2 0.326247 0.544111 0.881445 11.00000 -1.50000
AFIX 0
C29 1 0.435487 0.604783 0.793869 11.00000 0.00669 0.01929 =
0.01694 0.00201 0.00095 -0.00187
AFIX 13
H29 2 0.463083 0.649759 0.811167 11.00000 -1.20000
AFIX 0
C30 1 0.433874 0.588965 0.726748 11.00000 0.02518 0.01877 =
0.01704 0.01130 0.00781 0.01357
AFIX 137
H30A 2 0.404898 0.552436 0.706649 11.00000 -1.50000
H30B 2 0.461789 0.550592 0.723856 11.00000 -1.50000
H30C 2 0.433912 0.653822 0.707116 11.00000 -1.50000
AFIX 0
C31 1 0.447298 0.502517 0.826588 11.00000 0.01340 0.03222 =
0.02176 0.01096 0.01158 0.00644
AFIX 137
H31A 2 0.448524 0.510384 0.869428 11.00000 -1.50000
H31B 2 0.478184 0.478877 0.822803 11.00000 -1.50000
H31C 2 0.422615 0.453971 0.808109 11.00000 -1.50000
AFIX 0
C32 1 0.317707 0.810333 0.746408 11.00000 0.02304 0.02024 =
0.01611 0.01181 0.01285 0.00542
AFIX 23
H32A 2 0.320848 0.882607 0.755268 11.00000 -1.20000
H32B 2 0.302011 0.779019 0.775132 11.00000 -1.20000
AFIX 0
C33 1 0.287947 0.794203 0.682483 11.00000 0.01805 0.01886 =
0.02120 0.00386 0.00723 0.00580
AFIX 23
H33A 2 0.284647 0.721994 0.673462 11.00000 -1.20000
H33B 2 0.255786 0.822616 0.677382 11.00000 -1.20000
AFIX 0
O1 4 0.246213 1.114685 0.520487 11.00000 0.07076 0.08552 =
0.04377 0.00136 0.02434 0.00661
C34 1 0.200966 1.090867 0.494110 11.00000 0.04980 0.16963 =
0.05863 0.00760 0.02266 0.01880
AFIX 23
H34A 2 0.181092 1.151778 0.487702 11.00000 -1.20000
H34B 2 0.188901 1.045187 0.520539 11.00000 -1.20000
AFIX 0
C35 1 0.197932 1.041808 0.435110 11.00000 0.06439 0.09190 =
0.11301 -0.04088 0.03844 -0.04524
AFIX 23
H35A 2 0.177053 1.079946 0.401454 11.00000 -1.20000
H35B 2 0.185548 0.973010 0.434566 11.00000 -1.20000
AFIX 0
C36 1 0.249053 1.041575 0.430472 11.00000 0.04414 0.09120 =
0.04438 -0.01198 -0.00150 0.03807
AFIX 23
H36A 2 0.264609 0.976371 0.442384 11.00000 -1.20000
H36B 2 0.250874 1.058642 0.389174 11.00000 -1.20000
AFIX 0
C37 1 0.270384 1.121589 0.474893 11.00000 0.04321 0.07503 =
0.04055 0.01595 0.01576 -0.00963
AFIX 23
H37A 2 0.304912 1.110359 0.491838 11.00000 -1.20000
H37B 2 0.265549 1.188010 0.455433 11.00000 -1.20000
AFIX 0
HKLF 4
REM UDKING in C2/c #15
REM R1 = 0.0659 for 5310 Fo > 4sig(Fo) and 0.1027 for all 7597 data
REM 438 parameters refined using 33 restraints
END
WGHT 0.0264 24.2604
REM No hydrogen bonds found for HTAB generation
REM Highest difference peak 1.511, deepest hole -3.142, 1-sigma level 0.185
Q1 1 0.3699 0.8475 0.6815 11.00000 0.05 1.51
Q2 1 0.4419 0.8549 0.7098 11.00000 0.05 1.43
Q3 1 0.3785 0.8735 0.6865 11.00000 0.05 1.40
Q4 1 0.4270 0.8971 0.7012 11.00000 0.05 1.30
Q5 1 0.3655 0.8435 0.7324 11.00000 0.05 1.12
Q6 1 0.4067 0.8530 0.7282 11.00000 0.05 0.99
Q7 1 0.3810 0.7915 0.7275 11.00000 0.05 0.91
Q8 1 0.3684 0.8527 0.6379 11.00000 0.05 0.91
Q9 1 0.4459 0.8420 0.7566 11.00000 0.05 0.90
Q10 1 0.3757 0.8295 0.7374 11.00000 0.05 0.86
Q11 1 0.4070 0.8574 0.6694 11.00000 0.05 0.83
Q12 1 0.2340 0.9642 0.4591 11.00000 0.05 0.83
Q13 1 0.4153 0.9614 0.6585 11.00000 0.05 0.82
Q14 1 0.3473 0.7990 0.7522 11.00000 0.05 0.80
Q15 1 0.4819 0.7232 0.7440 11.00000 0.05 0.77
Q16 1 0.2224 0.9860 0.4891 11.00000 0.05 0.75
Q17 1 0.3335 0.8414 0.6578 11.00000 0.05 0.73
Q18 1 0.4082 1.1840 0.6974 11.00000 0.05 0.72
Q19 1 0.3441 0.7859 0.7388 11.00000 0.05 0.70
Q20 1 0.2762 1.2410 0.6722 11.00000 0.05 0.68
;
_shelx_res_checksum 52421
_olex2_submission_original_sample_id UDKING
_olex2_submission_special_instructions 'No special instructions were received'
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
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# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
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data_3
_database_code_depnum_ccdc_archive 'CCDC 1547174'
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_refine_special_details
;
Refined as a 2-component inversion twin.
;
_vrf_PLAT987_3
;
PROBLEM: The Flack x is >> 0 - Do a BASF/TWIN Refinement. Please Check.
RESPONSE: A BASF/TWIN refinement has been done.
;
_audit_creation_date 2016-03-18
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_shelx_SHELXL_version_number 2014/7
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C39 H93 N7 O P Si3 U'
_chemical_formula_sum 'C39 H93 N7 O P Si3 U'
_chemical_formula_weight 1029.47
_chemical_absolute_configuration ?
_chemical_melting_point ?
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'
P P 0.1023 0.0942 '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'
U U -9.6767 9.6646 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system orthorhombic
_space_group_IT_number 19
_space_group_name_H-M_alt 'P 21 21 21'
_space_group_name_Hall 'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
_cell_length_a 13.4366(5)
_cell_length_b 14.7631(5)
_cell_length_c 25.3924(9)
_cell_angle_alpha 90
_cell_angle_beta 90
_cell_angle_gamma 90
_cell_volume 5037.0(3)
_cell_formula_units_Z 4
_cell_measurement_reflns_used 10986
_cell_measurement_temperature 90(2)
_cell_measurement_theta_max 27.36
_cell_measurement_theta_min 2.21
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 3.360
_exptl_absorpt_correction_T_max 0.4305
_exptl_absorpt_correction_T_min 0.3693
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2007/2 (Bruker,2007) was used for absorption correction.
wR2(int) was 0.0550 before and 0.0310 after correction.
The Ratio of minimum to maximum transmission is 0.8578.
The \l/2 correction factor is 0.0015.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour purple
_exptl_crystal_density_diffrn 1.358
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2132
_exptl_crystal_size_max 0.33
_exptl_crystal_size_mid 0.32
_exptl_crystal_size_min 0.23
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0297
_diffrn_reflns_av_unetI/netI 0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -19
_diffrn_reflns_limit_l_max 32
_diffrn_reflns_limit_l_min -32
_diffrn_reflns_number 24682
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full 27.407
_diffrn_reflns_theta_max 27.407
_diffrn_reflns_theta_min 2.116
_diffrn_ambient_temperature 90(2)
_diffrn_detector 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 8.366
_diffrn_detector_type 'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method \w
_diffrn_radiation_monochromator graphite
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 40.0
_diffrn_source_power 2.0
_diffrn_source_type 'Incoatec I\ms'
_diffrn_source_voltage 50.0
_diffrn_special_details ?
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.816
_reflns_Friedel_fraction_full 0.997
_reflns_Friedel_fraction_max 0.997
_reflns_number_gt 10604
_reflns_number_total 11116
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'Bruker SAINT version 6.36A (Bruker, 2002)'
_computing_data_collection 'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction 'Bruker SAINT; SHELXTL (Sheldrick, 2008)'
_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 'SIR2004 (Burla et al., 2007)'
_refine_diff_density_max 1.546
_refine_diff_density_min -0.401
_refine_diff_density_rms 0.084
_refine_ls_abs_structure_details
;
Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack 0.346(4)
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 0.996
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 494
_refine_ls_number_reflns 11116
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0277
_refine_ls_R_factor_gt 0.0255
_refine_ls_restrained_S_all 0.996
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0258P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.0544
_refine_ls_wR_factor_ref 0.0552
_olex2_refinement_description
;
1. Twinned data refinement
Scales: 0.654(4) 0.346(4)
2. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
3.a Ternary CH refined with riding coordinates:
C12(H12), C23(H23), C1(H1), C29(H29), C26(H26), C15(H15), C18(H18), C4(H4),
C7(H7)
3.b Secondary CH2 refined with riding coordinates:
C11(H11a,H11b), C10(H10a,H10b), C22(H22a,H22b), C21(H21a,H21b), C33(H33a,
H33b), C32(H32a,H32b)
3.c Idealised Me refined as rotating group:
C24(H24a,H24b,H24c), C8(H8a,H8b,H8c), C39(H39a,H39b,H39c), C28(H28a,H28b,
H28c), C6(H6a,H6b,H6c), C35(H35a,H35b,H35c), C14(H14a,H14b,H14c), C30(H30a,
H30b,H30c), C31(H31a,H31b,H31c), C36(H36a,H36b,H36c), C16(H16a,H16b,H16c),
C25(H25a,H25b,H25c), C38(H38a,H38b,H38c), C17(H17a,H17b,H17c), C19(H19a,H19b,
H19c), C2(H2a,H2b,H2c), C9(H9a,H9b,H9c), C13(H13a,H13b,H13c), C5(H5a,H5b,H5c),
C34(H34a,H34b,H34c), C37(H37a,H37b,H37c), C20(H20a,H20b,H20c), C27(H27a,H27b,
H27c), C3(H3a,H3b,H3c)
;
_atom_sites_solution_hydrogens 'geom, Me from difmap'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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
U1 U 0.19431(2) 0.55693(2) 0.07239(2) 0.01368(5) Uani 1 1 d . . . . .
P1 P 0.28462(10) 0.35536(9) 0.16617(5) 0.0201(3) Uani 1 1 d . . . . .
Si2 Si 0.29223(11) 0.74052(9) 0.15780(5) 0.0179(3) Uani 1 1 d . . . . .
Si1 Si 0.33930(9) 0.45492(9) -0.03953(5) 0.0165(3) Uani 1 1 d . . . . .
Si3 Si -0.07321(10) 0.51025(9) 0.09367(5) 0.0156(3) Uani 1 1 d . . . . .
C12 C 0.1975(5) 0.6914(3) 0.20554(16) 0.0222(10) Uani 1 1 d . . . . .
H12 H 0.1897 0.6263 0.1954 0.027 Uiso 1 1 calc R . . . .
C23 C -0.1936(4) 0.5702(3) 0.11214(16) 0.0199(9) Uani 1 1 d . . . . .
H23 H -0.2171 0.5998 0.0790 0.024 Uiso 1 1 calc R . . . .
O1 O 0.2542(2) 0.4304(2) 0.12952(12) 0.0210(7) Uani 1 1 d . . . . .
C11 C 0.1788(4) 0.6637(3) -0.04930(16) 0.0181(10) Uani 1 1 d . . . . .
H11A H 0.2477 0.6864 -0.0537 0.022 Uiso 1 1 calc R . . . .
H11B H 0.1366 0.6919 -0.0767 0.022 Uiso 1 1 calc R . . . .
C24 C -0.1849(4) 0.6471(3) 0.15270(18) 0.0255(11) Uani 1 1 d . . . . .
H24A H -0.1712 0.6214 0.1875 0.038 Uiso 1 1 calc GR . . . .
H24B H -0.2475 0.6811 0.1538 0.038 Uiso 1 1 calc GR . . . .
H24C H -0.1306 0.6878 0.1426 0.038 Uiso 1 1 calc GR . . . .
N1 N 0.2438(3) 0.5198(3) -0.01541(15) 0.0175(8) Uani 1 1 d . . . . .
C10 C 0.1769(3) 0.5610(3) -0.05495(16) 0.0211(10) Uani 1 1 d . . . . .
H10A H 0.1082 0.5384 -0.0497 0.025 Uiso 1 1 calc R . . . .
H10B H 0.1988 0.5437 -0.0908 0.025 Uiso 1 1 calc R . . . .
N4 N 0.1410(3) 0.6878(3) 0.00374(14) 0.0150(8) Uani 1 1 d . . . . .
C1 C 0.4410(3) 0.4505(4) 0.01262(18) 0.0211(10) Uani 1 1 d . . . . .
H1 H 0.4094 0.4239 0.0447 0.025 Uiso 1 1 calc R . . . .
C29 C -0.1084(4) 0.4316(3) 0.03681(17) 0.0210(10) Uani 1 1 d . . . . .
H29 H -0.1548 0.3846 0.0509 0.025 Uiso 1 1 calc R . . . .
N3 N 0.0205(3) 0.5850(2) 0.07746(15) 0.0157(8) Uani 1 1 d . . . . .
C8 C 0.4602(4) 0.4351(4) -0.13477(18) 0.0253(11) Uani 1 1 d . . . . .
H8A H 0.5231 0.4335 -0.1152 0.038 Uiso 1 1 calc GR . . . .
H8B H 0.4724 0.4580 -0.1704 0.038 Uiso 1 1 calc GR . . . .
H8C H 0.4323 0.3739 -0.1368 0.038 Uiso 1 1 calc GR . . . .
C39 C 0.2185(4) 0.4462(4) 0.25014(18) 0.0312(12) Uani 1 1 d . . . . .
H39A H 0.1784 0.4745 0.2224 0.047 Uiso 1 1 calc GR . . . .
H39B H 0.2471 0.4933 0.2727 0.047 Uiso 1 1 calc GR . . . .
H39C H 0.1761 0.4063 0.2714 0.047 Uiso 1 1 calc GR . . . .
N7 N 0.2979(3) 0.3936(3) 0.22641(14) 0.0242(9) Uani 1 1 d . . . . .
C28 C -0.0781(4) 0.3427(4) 0.1533(2) 0.0273(12) Uani 1 1 d . . . . .
H28A H -0.1486 0.3516 0.1619 0.041 Uiso 1 1 calc GR . . . .
H28B H -0.0464 0.3067 0.1810 0.041 Uiso 1 1 calc GR . . . .
H28C H -0.0726 0.3109 0.1195 0.041 Uiso 1 1 calc GR . . . .
N2 N 0.2645(3) 0.6980(3) 0.09673(15) 0.0170(8) Uani 1 1 d . . . . .
C6 C 0.2161(4) 0.3266(4) -0.0929(2) 0.0316(13) Uani 1 1 d . . . . .
H6A H 0.1569 0.3584 -0.0801 0.047 Uiso 1 1 calc GR . . . .
H6B H 0.1998 0.2627 -0.0991 0.047 Uiso 1 1 calc GR . . . .
H6C H 0.2386 0.3543 -0.1259 0.047 Uiso 1 1 calc GR . . . .
C22 C 0.1862(4) 0.7743(3) 0.02176(17) 0.0183(9) Uani 1 1 d . . . . .
H22A H 0.1399 0.8058 0.0459 0.022 Uiso 1 1 calc R . . . .
H22B H 0.1985 0.8142 -0.0089 0.022 Uiso 1 1 calc R . . . .
C21 C 0.2834(3) 0.7547(3) 0.04987(18) 0.0179(10) Uani 1 1 d . . . . .
H21A H 0.3294 0.7228 0.0257 0.022 Uiso 1 1 calc R . . . .
H21B H 0.3151 0.8123 0.0607 0.022 Uiso 1 1 calc R . . . .
C35 C 0.4809(4) 0.3639(4) 0.1449(3) 0.0368(15) Uani 1 1 d . . . . .
H35A H 0.4628 0.4280 0.1413 0.055 Uiso 1 1 calc GR . . . .
H35B H 0.5185 0.3447 0.1138 0.055 Uiso 1 1 calc GR . . . .
H35C H 0.5219 0.3558 0.1764 0.055 Uiso 1 1 calc GR . . . .
C14 C 0.2314(4) 0.6910(4) 0.26372(19) 0.0313(13) Uani 1 1 d . . . . .
H14A H 0.2969 0.6621 0.2664 0.047 Uiso 1 1 calc GR . . . .
H14B H 0.1832 0.6571 0.2850 0.047 Uiso 1 1 calc GR . . . .
H14C H 0.2356 0.7534 0.2767 0.047 Uiso 1 1 calc GR . . . .
C30 C -0.0153(4) 0.3826(3) 0.0158(2) 0.0251(12) Uani 1 1 d . . . . .
H30A H 0.0316 0.4272 0.0016 0.038 Uiso 1 1 calc GR . . . .
H30B H -0.0347 0.3403 -0.0121 0.038 Uiso 1 1 calc GR . . . .
H30C H 0.0165 0.3491 0.0446 0.038 Uiso 1 1 calc GR . . . .
N5 N 0.3906(3) 0.3094(3) 0.14953(17) 0.0274(10) Uani 1 1 d . . . . .
C26 C -0.0264(4) 0.4352(4) 0.14922(17) 0.0198(10) Uani 1 1 d . . . . .
H26 H 0.0454 0.4226 0.1417 0.024 Uiso 1 1 calc R . . . .
C31 C -0.1615(4) 0.4804(4) -0.00864(19) 0.0262(12) Uani 1 1 d . . . . .
H31A H -0.2232 0.5079 0.0044 0.039 Uiso 1 1 calc GR . . . .
H31B H -0.1773 0.4366 -0.0365 0.039 Uiso 1 1 calc GR . . . .
H31C H -0.1180 0.5277 -0.0228 0.039 Uiso 1 1 calc GR . . . .
C36 C 0.1569(4) 0.2405(4) 0.1187(2) 0.0314(13) Uani 1 1 d . . . . .
H36A H 0.1648 0.2852 0.0905 0.047 Uiso 1 1 calc GR . . . .
H36B H 0.0860 0.2277 0.1239 0.047 Uiso 1 1 calc GR . . . .
H36C H 0.1916 0.1845 0.1090 0.047 Uiso 1 1 calc GR . . . .
C16 C 0.5009(4) 0.7358(4) 0.1434(2) 0.0255(12) Uani 1 1 d . . . . .
H16A H 0.4869 0.7149 0.1075 0.038 Uiso 1 1 calc GR . . . .
H16B H 0.5659 0.7126 0.1547 0.038 Uiso 1 1 calc GR . . . .
H16C H 0.5018 0.8022 0.1441 0.038 Uiso 1 1 calc GR . . . .
C33 C 0.0316(3) 0.6936(3) 0.00323(18) 0.0175(10) Uani 1 1 d . . . . .
H33A H 0.0045 0.6491 -0.0222 0.021 Uiso 1 1 calc R . . . .
H33B H 0.0110 0.7548 -0.0082 0.021 Uiso 1 1 calc R . . . .
C15 C 0.4196(4) 0.7007(3) 0.18093(18) 0.0221(11) Uani 1 1 d . . . . .
H15 H 0.4323 0.7256 0.2169 0.027 Uiso 1 1 calc R . . . .
C25 C -0.2785(4) 0.5047(4) 0.1284(2) 0.0286(12) Uani 1 1 d . . . . .
H25A H -0.2855 0.4571 0.1018 0.043 Uiso 1 1 calc GR . . . .
H25B H -0.3410 0.5385 0.1313 0.043 Uiso 1 1 calc GR . . . .
H25C H -0.2625 0.4772 0.1625 0.043 Uiso 1 1 calc GR . . . .
C18 C 0.2997(4) 0.8705(3) 0.15982(18) 0.0240(10) Uani 1 1 d . . . . .
H18 H 0.3572 0.8875 0.1369 0.029 Uiso 1 1 calc R . . . .
C38 C 0.3683(4) 0.3578(4) 0.2645(2) 0.0381(15) Uani 1 1 d . . . . .
H38A H 0.3320 0.3290 0.2935 0.057 Uiso 1 1 calc GR . . . .
H38B H 0.4092 0.4073 0.2783 0.057 Uiso 1 1 calc GR . . . .
H38C H 0.4112 0.3129 0.2474 0.057 Uiso 1 1 calc GR . . . .
C17 C 0.4258(4) 0.5976(4) 0.1832(2) 0.0265(12) Uani 1 1 d . . . . .
H17A H 0.3772 0.5747 0.2088 0.040 Uiso 1 1 calc GR . . . .
H17B H 0.4929 0.5794 0.1940 0.040 Uiso 1 1 calc GR . . . .
H17C H 0.4112 0.5724 0.1484 0.040 Uiso 1 1 calc GR . . . .
C19 C 0.3246(5) 0.9063(4) 0.2149(2) 0.0392(15) Uani 1 1 d . . . . .
H19A H 0.2691 0.8937 0.2388 0.059 Uiso 1 1 calc GR . . . .
H19B H 0.3359 0.9719 0.2131 0.059 Uiso 1 1 calc GR . . . .
H19C H 0.3849 0.8764 0.2279 0.059 Uiso 1 1 calc GR . . . .
C32 C -0.0101(3) 0.6744(3) 0.05778(17) 0.0174(10) Uani 1 1 d . . . . .
H32A H 0.0133 0.7217 0.0825 0.021 Uiso 1 1 calc R . . . .
H32B H -0.0836 0.6773 0.0565 0.021 Uiso 1 1 calc R . . . .
C2 C 0.5284(4) 0.3888(4) -0.0011(2) 0.0307(13) Uani 1 1 d . . . . .
H2A H 0.5035 0.3282 -0.0097 0.046 Uiso 1 1 calc GR . . . .
H2B H 0.5736 0.3850 0.0291 0.046 Uiso 1 1 calc GR . . . .
H2C H 0.5642 0.4136 -0.0314 0.046 Uiso 1 1 calc GR . . . .
C9 C 0.4281(4) 0.5943(3) -0.1057(2) 0.0305(13) Uani 1 1 d . . . . .
H9A H 0.3809 0.6347 -0.0880 0.046 Uiso 1 1 calc GR . . . .
H9B H 0.4385 0.6150 -0.1420 0.046 Uiso 1 1 calc GR . . . .
H9C H 0.4917 0.5949 -0.0868 0.046 Uiso 1 1 calc GR . . . .
C13 C 0.0942(4) 0.7331(4) 0.2008(2) 0.0290(12) Uani 1 1 d . . . . .
H13A H 0.0968 0.7968 0.2115 0.044 Uiso 1 1 calc GR . . . .
H13B H 0.0478 0.7003 0.2235 0.044 Uiso 1 1 calc GR . . . .
H13C H 0.0717 0.7292 0.1641 0.044 Uiso 1 1 calc GR . . . .
C5 C 0.2631(4) 0.2899(3) -0.0007(2) 0.0263(12) Uani 1 1 d . . . . .
H5A H 0.3182 0.2871 0.0245 0.039 Uiso 1 1 calc GR . . . .
H5B H 0.2391 0.2284 -0.0079 0.039 Uiso 1 1 calc GR . . . .
H5C H 0.2088 0.3261 0.0142 0.039 Uiso 1 1 calc GR . . . .
C34 C 0.4105(5) 0.2124(4) 0.1496(3) 0.0479(17) Uani 1 1 d . . . . .
H34A H 0.4549 0.1976 0.1790 0.072 Uiso 1 1 calc GR . . . .
H34B H 0.4422 0.1952 0.1164 0.072 Uiso 1 1 calc GR . . . .
H34C H 0.3478 0.1793 0.1536 0.072 Uiso 1 1 calc GR . . . .
N6 N 0.1991(4) 0.2760(3) 0.16723(15) 0.0247(9) Uani 1 1 d . . . . .
C4 C 0.2990(4) 0.3332(3) -0.05166(17) 0.0222(10) Uani 1 1 d . . . . .
H4 H 0.3578 0.2983 -0.0647 0.027 Uiso 1 1 calc R . . . .
C37 C 0.1827(6) 0.2172(4) 0.2128(2) 0.0404(15) Uani 1 1 d . . . . .
H37A H 0.2145 0.1584 0.2066 0.061 Uiso 1 1 calc GR . . . .
H37B H 0.1111 0.2084 0.2181 0.061 Uiso 1 1 calc GR . . . .
H37C H 0.2116 0.2453 0.2443 0.061 Uiso 1 1 calc GR . . . .
C20 C 0.2106(4) 0.9232(3) 0.1388(2) 0.0301(13) Uani 1 1 d . . . . .
H20A H 0.1968 0.9043 0.1025 0.045 Uiso 1 1 calc GR . . . .
H20B H 0.2254 0.9881 0.1395 0.045 Uiso 1 1 calc GR . . . .
H20C H 0.1522 0.9109 0.1608 0.045 Uiso 1 1 calc GR . . . .
C27 C -0.0300(4) 0.4814(4) 0.20324(18) 0.0255(12) Uani 1 1 d . . . . .
H27A H 0.0026 0.5407 0.2011 0.038 Uiso 1 1 calc GR . . . .
H27B H 0.0045 0.4437 0.2292 0.038 Uiso 1 1 calc GR . . . .
H27C H -0.0995 0.4895 0.2140 0.038 Uiso 1 1 calc GR . . . .
C7 C 0.3864(4) 0.4980(3) -0.10633(19) 0.0209(11) Uani 1 1 d . . . . .
H7 H 0.3263 0.5006 -0.1295 0.025 Uiso 1 1 calc R . . . .
C3 C 0.4804(4) 0.5435(4) 0.0291(2) 0.0291(12) Uani 1 1 d . . . . .
H3A H 0.5149 0.5717 -0.0006 0.044 Uiso 1 1 calc GR . . . .
H3B H 0.5269 0.5363 0.0586 0.044 Uiso 1 1 calc GR . . . .
H3C H 0.4247 0.5820 0.0401 0.044 Uiso 1 1 calc GR . . . .
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
U1 0.01304(7) 0.01377(7) 0.01424(7) 0.00069(7) -0.00081(7) 0.00078(7)
P1 0.0192(8) 0.0212(7) 0.0199(6) 0.0059(5) -0.0011(5) 0.0022(5)
Si2 0.0155(7) 0.0208(7) 0.0175(6) -0.0032(5) -0.0003(6) -0.0003(6)
Si1 0.0161(6) 0.0152(7) 0.0182(5) -0.0021(5) 0.0013(5) 0.0000(5)
Si3 0.0141(6) 0.0161(6) 0.0165(5) 0.0005(5) 0.0004(5) -0.0012(5)
C12 0.023(3) 0.028(3) 0.016(2) -0.0014(18) 0.000(2) -0.001(3)
C23 0.014(2) 0.027(3) 0.0183(18) 0.0016(18) 0.000(2) 0.001(2)
O1 0.0199(18) 0.021(2) 0.0225(15) 0.0040(15) -0.0009(13) 0.0005(15)
C11 0.016(3) 0.022(2) 0.0167(19) 0.0039(18) 0.0003(19) 0.005(2)
C24 0.022(3) 0.031(3) 0.023(2) -0.006(2) 0.005(2) 0.005(3)
N1 0.017(2) 0.018(2) 0.0174(18) -0.0006(16) -0.0019(16) 0.0036(17)
C10 0.020(3) 0.028(3) 0.0155(18) -0.003(2) -0.0010(17) 0.003(2)
N4 0.012(2) 0.016(2) 0.0167(18) 0.0003(16) -0.0002(16) 0.0001(16)
C1 0.019(2) 0.020(3) 0.024(2) -0.001(2) -0.0001(19) 0.004(2)
C29 0.022(3) 0.017(3) 0.024(2) -0.002(2) 0.0005(19) -0.004(2)
N3 0.0152(19) 0.0120(18) 0.0200(18) -0.0004(15) -0.0030(17) -0.0015(14)
C8 0.028(3) 0.025(3) 0.023(2) -0.006(2) 0.008(2) -0.004(3)
C39 0.033(3) 0.037(3) 0.024(2) 0.002(3) 0.005(2) 0.007(3)
N7 0.022(2) 0.030(2) 0.0208(18) 0.0062(16) -0.002(2) 0.003(2)
C28 0.034(3) 0.021(3) 0.026(2) 0.006(2) 0.001(2) -0.004(3)
N2 0.014(2) 0.019(2) 0.0179(18) -0.0001(16) -0.0004(16) -0.0011(16)
C6 0.037(4) 0.028(3) 0.029(2) -0.008(2) 0.005(2) -0.012(3)
C22 0.019(2) 0.016(2) 0.020(2) 0.0018(17) 0.002(2) 0.000(2)
C21 0.015(3) 0.017(2) 0.022(2) -0.0019(18) 0.0021(19) -0.0022(19)
C35 0.019(3) 0.042(4) 0.050(4) 0.013(3) 0.001(3) 0.005(3)
C14 0.025(3) 0.045(4) 0.023(2) -0.002(2) 0.004(2) 0.001(3)
C30 0.030(3) 0.018(3) 0.027(3) -0.002(2) 0.002(2) 0.003(2)
N5 0.021(2) 0.025(3) 0.036(2) 0.010(2) 0.004(2) 0.0060(19)
C26 0.016(2) 0.021(3) 0.022(2) 0.004(2) -0.0006(19) -0.004(2)
C31 0.032(3) 0.024(3) 0.022(2) -0.002(2) -0.007(2) -0.002(2)
C36 0.033(3) 0.033(3) 0.028(3) 0.007(2) -0.002(2) -0.008(3)
C16 0.019(3) 0.033(3) 0.024(2) -0.005(2) -0.001(2) -0.002(2)
C33 0.013(2) 0.019(3) 0.021(2) 0.0002(19) -0.0020(19) -0.001(2)
C15 0.020(3) 0.029(3) 0.017(2) -0.004(2) -0.001(2) -0.001(2)
C25 0.017(3) 0.040(3) 0.029(3) 0.000(2) 0.001(2) -0.001(2)
C18 0.021(3) 0.023(3) 0.028(2) -0.0052(19) 0.000(3) -0.001(2)
C38 0.032(3) 0.054(4) 0.028(3) 0.008(3) -0.009(3) 0.004(3)
C17 0.021(3) 0.029(3) 0.029(3) 0.002(2) 0.003(2) 0.005(2)
C19 0.041(4) 0.032(3) 0.044(3) -0.015(3) -0.008(3) 0.000(3)
C32 0.013(2) 0.014(2) 0.024(2) -0.0008(19) 0.0024(18) -0.0001(19)
C2 0.025(3) 0.029(3) 0.039(3) -0.006(2) -0.006(3) 0.013(3)
C9 0.031(3) 0.021(3) 0.039(3) -0.002(2) 0.016(3) -0.001(2)
C13 0.021(3) 0.041(3) 0.025(2) -0.004(2) 0.003(2) -0.001(3)
C5 0.027(3) 0.018(3) 0.034(3) 0.000(2) 0.007(2) -0.001(2)
C34 0.033(4) 0.036(4) 0.074(5) -0.004(3) 0.002(4) 0.011(3)
N6 0.028(2) 0.024(2) 0.0214(18) 0.0058(16) -0.002(2) -0.003(2)
C4 0.023(3) 0.016(2) 0.028(2) -0.0048(19) 0.009(2) -0.004(2)
C37 0.052(4) 0.038(3) 0.032(3) 0.012(3) 0.001(3) -0.010(3)
C20 0.029(3) 0.022(3) 0.039(3) -0.006(2) 0.000(2) 0.001(2)
C27 0.027(3) 0.031(3) 0.018(2) 0.003(2) -0.004(2) -0.001(2)
C7 0.019(3) 0.020(3) 0.024(2) -0.003(2) 0.001(2) -0.001(2)
C3 0.024(3) 0.026(3) 0.038(3) -0.009(2) -0.012(2) 0.001(2)
_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
U1 O1 2.498(3) . ?
U1 N1 2.390(4) . ?
U1 N4 2.699(4) . ?
U1 N3 2.375(4) . ?
U1 N2 2.369(4) . ?
P1 O1 1.504(3) . ?
P1 N7 1.640(4) . ?
P1 N5 1.633(5) . ?
P1 N6 1.641(5) . ?
Si2 C12 1.901(5) . ?
Si2 N2 1.714(4) . ?
Si2 C15 1.903(5) . ?
Si2 C18 1.921(5) . ?
Si1 N1 1.715(4) . ?
Si1 C1 1.904(5) . ?
Si1 C4 1.902(5) . ?
Si1 C7 1.919(5) . ?
Si3 C23 1.902(5) . ?
Si3 C29 1.912(5) . ?
Si3 N3 1.724(4) . ?
Si3 C26 1.901(5) . ?
C12 H12 1.0000 . ?
C12 C14 1.546(6) . ?
C12 C13 1.524(8) . ?
C23 H23 1.0000 . ?
C23 C24 1.538(6) . ?
C23 C25 1.551(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C10 1.524(7) . ?
C11 N4 1.483(5) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
N1 C10 1.478(6) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
N4 C22 1.486(6) . ?
N4 C33 1.472(6) . ?
C1 H1 1.0000 . ?
C1 C2 1.527(7) . ?
C1 C3 1.530(7) . ?
C29 H29 1.0000 . ?
C29 C30 1.540(7) . ?
C29 C31 1.536(7) . ?
N3 C32 1.471(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C8 C7 1.539(7) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 N7 1.451(6) . ?
N7 C38 1.453(6) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C26 1.535(7) . ?
N2 C21 1.477(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C6 C4 1.532(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.517(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C35 N5 1.461(7) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
N5 C34 1.457(7) . ?
C26 H26 1.0000 . ?
C26 C27 1.533(6) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C36 N6 1.455(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 C15 1.539(7) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C32 1.520(6) . ?
C15 H15 1.0000 . ?
C15 C17 1.527(7) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C18 H18 1.0000 . ?
C18 C19 1.532(7) . ?
C18 C20 1.525(7) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C9 C7 1.527(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C5 C4 1.522(7) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
N6 C37 1.464(6) . ?
C4 H4 1.0000 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C7 H7 1.0000 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 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
O1 U1 N4 174.73(11) . . ?
N1 U1 O1 106.31(12) . . ?
N1 U1 N4 68.62(12) . . ?
N3 U1 O1 114.54(11) . . ?
N3 U1 N1 111.36(13) . . ?
N3 U1 N4 69.47(12) . . ?
N2 U1 O1 112.20(12) . . ?
N2 U1 N1 109.52(13) . . ?
N2 U1 N4 69.19(12) . . ?
N2 U1 N3 102.94(13) . . ?
O1 P1 N7 110.7(2) . . ?
O1 P1 N5 112.5(2) . . ?
O1 P1 N6 110.2(2) . . ?
N7 P1 N6 107.8(2) . . ?
N5 P1 N7 106.8(2) . . ?
N5 P1 N6 108.6(2) . . ?
C12 Si2 C15 106.7(2) . . ?
C12 Si2 C18 113.5(2) . . ?
N2 Si2 C12 107.0(2) . . ?
N2 Si2 C15 111.2(2) . . ?
N2 Si2 C18 113.6(2) . . ?
C15 Si2 C18 104.7(2) . . ?
N1 Si1 C1 107.9(2) . . ?
N1 Si1 C4 111.9(2) . . ?
N1 Si1 C7 112.1(2) . . ?
C1 Si1 C7 112.9(2) . . ?
C4 Si1 C1 106.6(2) . . ?
C4 Si1 C7 105.3(2) . . ?
C23 Si3 C29 105.0(2) . . ?
N3 Si3 C23 112.5(2) . . ?
N3 Si3 C29 112.9(2) . . ?
N3 Si3 C26 107.9(2) . . ?
C26 Si3 C23 111.7(2) . . ?
C26 Si3 C29 106.7(2) . . ?
Si2 C12 H12 105.8 . . ?
C14 C12 Si2 114.5(4) . . ?
C14 C12 H12 105.8 . . ?
C13 C12 Si2 113.9(3) . . ?
C13 C12 H12 105.8 . . ?
C13 C12 C14 110.2(4) . . ?
Si3 C23 H23 105.3 . . ?
C24 C23 Si3 116.4(4) . . ?
C24 C23 H23 105.3 . . ?
C24 C23 C25 109.7(4) . . ?
C25 C23 Si3 113.7(3) . . ?
C25 C23 H23 105.3 . . ?
P1 O1 U1 176.3(2) . . ?
H11A C11 H11B 108.4 . . ?
C10 C11 H11A 110.0 . . ?
C10 C11 H11B 110.0 . . ?
N4 C11 H11A 110.0 . . ?
N4 C11 H11B 110.0 . . ?
N4 C11 C10 108.6(4) . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si1 N1 U1 132.0(2) . . ?
C10 N1 U1 111.7(3) . . ?
C10 N1 Si1 116.2(3) . . ?
C11 C10 H10A 109.8 . . ?
C11 C10 H10B 109.8 . . ?
N1 C10 C11 109.6(4) . . ?
N1 C10 H10A 109.8 . . ?
N1 C10 H10B 109.8 . . ?
H10A C10 H10B 108.2 . . ?
C11 N4 U1 108.9(3) . . ?
C11 N4 C22 110.2(4) . . ?
C22 N4 U1 107.9(3) . . ?
C33 N4 U1 108.2(3) . . ?
C33 N4 C11 110.4(4) . . ?
C33 N4 C22 111.2(4) . . ?
Si1 C1 H1 106.1 . . ?
C2 C1 Si1 114.5(3) . . ?
C2 C1 H1 106.1 . . ?
C2 C1 C3 109.4(4) . . ?
C3 C1 Si1 114.1(4) . . ?
C3 C1 H1 106.1 . . ?
Si3 C29 H29 107.7 . . ?
C30 C29 Si3 110.2(3) . . ?
C30 C29 H29 107.7 . . ?
C31 C29 Si3 113.4(3) . . ?
C31 C29 H29 107.7 . . ?
C31 C29 C30 109.7(4) . . ?
Si3 N3 U1 128.31(19) . . ?
C32 N3 U1 114.4(3) . . ?
C32 N3 Si3 116.8(3) . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
N7 C39 H39A 109.5 . . ?
N7 C39 H39B 109.5 . . ?
N7 C39 H39C 109.5 . . ?
C39 N7 P1 119.5(3) . . ?
C39 N7 C38 113.4(4) . . ?
C38 N7 P1 124.5(4) . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
Si2 N2 U1 130.1(2) . . ?
C21 N2 U1 110.9(3) . . ?
C21 N2 Si2 119.0(3) . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
N4 C22 H22A 109.8 . . ?
N4 C22 H22B 109.8 . . ?
N4 C22 C21 109.5(4) . . ?
H22A C22 H22B 108.2 . . ?
C21 C22 H22A 109.8 . . ?
C21 C22 H22B 109.8 . . ?
N2 C21 C22 109.8(4) . . ?
N2 C21 H21A 109.7 . . ?
N2 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
H35A C35 H35B 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
N5 C35 H35A 109.5 . . ?
N5 C35 H35B 109.5 . . ?
N5 C35 H35C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C35 N5 P1 121.1(4) . . ?
C34 N5 P1 124.6(4) . . ?
C34 N5 C35 112.9(5) . . ?
Si3 C26 H26 106.6 . . ?
C28 C26 Si3 114.7(3) . . ?
C28 C26 H26 106.6 . . ?
C27 C26 Si3 113.1(4) . . ?
C27 C26 C28 108.8(4) . . ?
C27 C26 H26 106.6 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N6 C36 H36A 109.5 . . ?
N6 C36 H36B 109.5 . . ?
N6 C36 H36C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
N4 C33 H33A 109.6 . . ?
N4 C33 H33B 109.6 . . ?
N4 C33 C32 110.4(4) . . ?
H33A C33 H33B 108.1 . . ?
C32 C33 H33A 109.6 . . ?
C32 C33 H33B 109.6 . . ?
Si2 C15 H15 108.8 . . ?
C16 C15 Si2 110.1(3) . . ?
C16 C15 H15 108.8 . . ?
C17 C15 Si2 111.6(4) . . ?
C17 C15 C16 108.7(4) . . ?
C17 C15 H15 108.8 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si2 C18 H18 106.0 . . ?
C19 C18 Si2 112.4(4) . . ?
C19 C18 H18 106.0 . . ?
C20 C18 Si2 117.3(4) . . ?
C20 C18 H18 106.0 . . ?
C20 C18 C19 108.4(4) . . ?
N7 C38 H38A 109.5 . . ?
N7 C38 H38B 109.5 . . ?
N7 C38 H38C 109.5 . . ?
H38A C38 H38B 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N3 C32 C33 111.9(4) . . ?
N3 C32 H32A 109.2 . . ?
N3 C32 H32B 109.2 . . ?
C33 C32 H32A 109.2 . . ?
C33 C32 H32B 109.2 . . ?
H32A C32 H32B 107.9 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
N5 C34 H34A 109.5 . . ?
N5 C34 H34B 109.5 . . ?
N5 C34 H34C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C36 N6 P1 121.1(3) . . ?
C36 N6 C37 113.4(4) . . ?
C37 N6 P1 122.8(4) . . ?
Si1 C4 H4 108.4 . . ?
C6 C4 Si1 112.2(3) . . ?
C6 C4 H4 108.4 . . ?
C5 C4 Si1 110.5(3) . . ?
C5 C4 C6 108.9(4) . . ?
C5 C4 H4 108.4 . . ?
N6 C37 H37A 109.5 . . ?
N6 C37 H37B 109.5 . . ?
N6 C37 H37C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
Si1 C7 H7 105.5 . . ?
C8 C7 Si1 115.3(4) . . ?
C8 C7 H7 105.5 . . ?
C9 C7 Si1 114.9(3) . . ?
C9 C7 C8 109.2(4) . . ?
C9 C7 H7 105.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 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
U1 N1 C10 C11 60.2(4) . . . . ?
U1 N4 C22 C21 30.7(4) . . . . ?
U1 N4 C33 C32 34.6(4) . . . . ?
U1 N3 C32 C33 50.9(4) . . . . ?
U1 N2 C21 C22 61.6(4) . . . . ?
Si2 N2 C21 C22 -117.4(4) . . . . ?
Si1 N1 C10 C11 -120.5(3) . . . . ?
Si3 N3 C32 C33 -121.8(4) . . . . ?
C12 Si2 N2 U1 -31.5(3) . . . . ?
C12 Si2 N2 C21 147.3(3) . . . . ?
C23 Si3 N3 U1 163.0(2) . . . . ?
C23 Si3 N3 C32 -25.5(4) . . . . ?
O1 P1 N7 C39 51.1(5) . . . . ?
O1 P1 N7 C38 -148.5(4) . . . . ?
O1 P1 N5 C35 57.2(5) . . . . ?
O1 P1 N5 C34 -137.2(5) . . . . ?
O1 P1 N6 C36 47.5(5) . . . . ?
O1 P1 N6 C37 -152.3(4) . . . . ?
C11 N4 C22 C21 -88.1(4) . . . . ?
C11 N4 C33 C32 153.7(4) . . . . ?
C10 C11 N4 U1 33.2(4) . . . . ?
C10 C11 N4 C22 151.4(4) . . . . ?
C10 C11 N4 C33 -85.4(4) . . . . ?
N4 C11 C10 N1 -62.2(5) . . . . ?
N4 C22 C21 N2 -61.6(5) . . . . ?
N4 C33 C32 N3 -57.7(5) . . . . ?
C1 Si1 N1 U1 -23.7(4) . . . . ?
C1 Si1 N1 C10 157.2(3) . . . . ?
C29 Si3 N3 U1 -78.5(3) . . . . ?
C29 Si3 N3 C32 93.1(3) . . . . ?
N7 P1 N5 C35 -64.4(5) . . . . ?
N7 P1 N5 C34 101.1(5) . . . . ?
N7 P1 N6 C36 168.4(4) . . . . ?
N7 P1 N6 C37 -31.4(5) . . . . ?
C22 N4 C33 C32 -83.7(4) . . . . ?
N5 P1 N7 C39 174.0(4) . . . . ?
N5 P1 N7 C38 -25.7(5) . . . . ?
N5 P1 N6 C36 -76.1(5) . . . . ?
N5 P1 N6 C37 84.0(5) . . . . ?
C26 Si3 N3 U1 39.3(3) . . . . ?
C26 Si3 N3 C32 -149.2(3) . . . . ?
C33 N4 C22 C21 149.2(4) . . . . ?
C15 Si2 N2 U1 84.7(3) . . . . ?
C15 Si2 N2 C21 -96.6(4) . . . . ?
C18 Si2 N2 U1 -157.5(3) . . . . ?
C18 Si2 N2 C21 21.2(4) . . . . ?
N6 P1 N7 C39 -69.5(4) . . . . ?
N6 P1 N7 C38 90.9(5) . . . . ?
N6 P1 N5 C35 179.5(4) . . . . ?
N6 P1 N5 C34 -14.9(5) . . . . ?
C4 Si1 N1 U1 93.2(3) . . . . ?
C4 Si1 N1 C10 -85.9(4) . . . . ?
C7 Si1 N1 U1 -148.7(3) . . . . ?
C7 Si1 N1 C10 32.2(4) . . . . ?
_shelx_res_file
;
udkinq.res created by SHELXL-2014/7
TITL UDKINQ in P212121 for DMK/STL
REM reset to P212121 #19
rem EXTI insignif
CELL 0.71073 13.4366 14.7631 25.3924 90 90 90
ZERR 4 0.0005 0.0005 0.0009 0 0 0
LATT -1
SYMM 0.5-X,-Y,0.5+Z
SYMM 0.5+X,0.5-Y,-Z
SYMM -X,0.5+Y,0.5-Z
SFAC C H N O P Si U
UNIT 156 372 28 4 4 12 4
L.S. 16
PLAN 20
TEMP -183(2)
BOND $H
HTAB
CONF
MORE -1
fmap 2
acta 55
TWIN -1 0 0 0 -1 0 0 0 -1 2
OMIT 2 2 1
REM
REM
REM
WGHT 0.025800
BASF 0.34645
FVAR 0.06845
U1 7 0.194309 0.556931 0.072387 11.00000 0.01304 0.01377 =
0.01424 0.00069 -0.00081 0.00078
P1 5 0.284616 0.355360 0.166166 11.00000 0.01922 0.02117 =
0.01988 0.00592 -0.00113 0.00224
SI2 6 0.292233 0.740525 0.157797 11.00000 0.01551 0.02080 =
0.01746 -0.00318 -0.00027 -0.00031
SI1 6 0.339302 0.454923 -0.039532 11.00000 0.01612 0.01523 =
0.01818 -0.00206 0.00130 0.00004
SI3 6 -0.073212 0.510253 0.093672 11.00000 0.01412 0.01607 =
0.01648 0.00051 0.00042 -0.00118
C12 1 0.197543 0.691402 0.205543 11.00000 0.02260 0.02766 =
0.01638 -0.00137 0.00016 -0.00125
AFIX 13
H12 2 0.189741 0.626331 0.195412 11.00000 -1.20000
AFIX 0
C23 1 -0.193588 0.570175 0.112144 11.00000 0.01433 0.02706 =
0.01828 0.00159 0.00026 0.00060
AFIX 13
H23 2 -0.217112 0.599808 0.078991 11.00000 -1.20000
AFIX 0
O1 4 0.254174 0.430419 0.129523 11.00000 0.01995 0.02052 =
0.02253 0.00403 -0.00093 0.00047
C11 1 0.178835 0.663723 -0.049302 11.00000 0.01587 0.02162 =
0.01674 0.00394 0.00035 0.00516
AFIX 23
H11A 2 0.247679 0.686392 -0.053692 11.00000 -1.20000
H11B 2 0.136574 0.691854 -0.076733 11.00000 -1.20000
AFIX 0
C24 1 -0.184929 0.647114 0.152703 11.00000 0.02196 0.03142 =
0.02311 -0.00565 0.00521 0.00507
AFIX 137
H24A 2 -0.171201 0.621449 0.187547 11.00000 -1.50000
H24B 2 -0.247515 0.681144 0.153831 11.00000 -1.50000
H24C 2 -0.130552 0.687784 0.142581 11.00000 -1.50000
AFIX 0
N1 3 0.243828 0.519841 -0.015406 11.00000 0.01740 0.01777 =
0.01745 -0.00059 -0.00189 0.00359
C10 1 0.176918 0.560966 -0.054948 11.00000 0.02007 0.02780 =
0.01553 -0.00325 -0.00099 0.00314
AFIX 23
H10A 2 0.108235 0.538404 -0.049743 11.00000 -1.20000
H10B 2 0.198791 0.543677 -0.090796 11.00000 -1.20000
AFIX 0
N4 3 0.140981 0.687805 0.003738 11.00000 0.01201 0.01636 =
0.01673 0.00032 -0.00023 0.00012
C1 1 0.440970 0.450537 0.012622 11.00000 0.01885 0.02032 =
0.02416 -0.00051 -0.00010 0.00434
AFIX 13
H1 2 0.409423 0.423852 0.044740 11.00000 -1.20000
AFIX 0
C29 1 -0.108385 0.431618 0.036813 11.00000 0.02213 0.01719 =
0.02354 -0.00156 0.00051 -0.00384
AFIX 13
H29 2 -0.154832 0.384602 0.050942 11.00000 -1.20000
AFIX 0
N3 3 0.020547 0.584954 0.077462 11.00000 0.01519 0.01197 =
0.01999 -0.00044 -0.00297 -0.00152
C8 1 0.460239 0.435149 -0.134766 11.00000 0.02773 0.02528 =
0.02275 -0.00584 0.00843 -0.00426
AFIX 137
H8A 2 0.523101 0.433485 -0.115218 11.00000 -1.50000
H8B 2 0.472369 0.457985 -0.170432 11.00000 -1.50000
H8C 2 0.432286 0.373932 -0.136756 11.00000 -1.50000
AFIX 0
C39 1 0.218454 0.446192 0.250141 11.00000 0.03256 0.03704 =
0.02406 0.00157 0.00506 0.00665
AFIX 137
H39A 2 0.178440 0.474521 0.222394 11.00000 -1.50000
H39B 2 0.247146 0.493292 0.272705 11.00000 -1.50000
H39C 2 0.176135 0.406296 0.271355 11.00000 -1.50000
AFIX 0
N7 3 0.297853 0.393594 0.226413 11.00000 0.02158 0.03021 =
0.02079 0.00619 -0.00250 0.00297
C28 1 -0.078142 0.342726 0.153271 11.00000 0.03431 0.02119 =
0.02637 0.00608 0.00126 -0.00358
AFIX 137
H28A 2 -0.148561 0.351628 0.161886 11.00000 -1.50000
H28B 2 -0.046361 0.306674 0.180972 11.00000 -1.50000
H28C 2 -0.072561 0.310870 0.119540 11.00000 -1.50000
AFIX 0
N2 3 0.264471 0.698029 0.096733 11.00000 0.01380 0.01917 =
0.01792 -0.00012 -0.00039 -0.00105
C6 1 0.216120 0.326560 -0.092922 11.00000 0.03699 0.02849 =
0.02925 -0.00782 0.00486 -0.01216
AFIX 137
H6A 2 0.156868 0.358425 -0.080147 11.00000 -1.50000
H6B 2 0.199843 0.262734 -0.099112 11.00000 -1.50000
H6C 2 0.238644 0.354277 -0.125903 11.00000 -1.50000
AFIX 0
C22 1 0.186164 0.774273 0.021758 11.00000 0.01882 0.01603 =
0.01991 0.00185 0.00156 -0.00030
AFIX 23
H22A 2 0.139914 0.805795 0.045949 11.00000 -1.20000
H22B 2 0.198547 0.814210 -0.008869 11.00000 -1.20000
AFIX 0
C21 1 0.283415 0.754679 0.049867 11.00000 0.01499 0.01721 =
0.02158 -0.00189 0.00213 -0.00224
AFIX 23
H21A 2 0.329416 0.722759 0.025719 11.00000 -1.20000
H21B 2 0.315103 0.812291 0.060681 11.00000 -1.20000
AFIX 0
C35 1 0.480893 0.363948 0.144879 11.00000 0.01858 0.04218 =
0.04965 0.01318 0.00053 0.00513
AFIX 137
H35A 2 0.462833 0.427967 0.141303 11.00000 -1.50000
H35B 2 0.518516 0.344656 0.113776 11.00000 -1.50000
H35C 2 0.521905 0.355804 0.176440 11.00000 -1.50000
AFIX 0
C14 1 0.231401 0.690950 0.263724 11.00000 0.02510 0.04547 =
0.02325 -0.00220 0.00421 0.00053
AFIX 137
H14A 2 0.296897 0.662119 0.266436 11.00000 -1.50000
H14B 2 0.183185 0.657074 0.284952 11.00000 -1.50000
H14C 2 0.235585 0.753372 0.276667 11.00000 -1.50000
AFIX 0
C30 1 -0.015319 0.382606 0.015833 11.00000 0.03048 0.01841 =
0.02652 -0.00242 0.00248 0.00279
AFIX 137
H30A 2 0.031558 0.427221 0.001643 11.00000 -1.50000
H30B 2 -0.034742 0.340320 -0.012085 11.00000 -1.50000
H30C 2 0.016458 0.349085 0.044590 11.00000 -1.50000
AFIX 0
N5 3 0.390608 0.309419 0.149525 11.00000 0.02092 0.02522 =
0.03593 0.01039 0.00388 0.00596
C26 1 -0.026361 0.435156 0.149221 11.00000 0.01642 0.02103 =
0.02184 0.00354 -0.00058 -0.00352
AFIX 13
H26 2 0.045372 0.422609 0.141677 11.00000 -1.20000
AFIX 0
C31 1 -0.161512 0.480372 -0.008643 11.00000 0.03219 0.02421 =
0.02205 -0.00198 -0.00703 -0.00231
AFIX 137
H31A 2 -0.223165 0.507869 0.004380 11.00000 -1.50000
H31B 2 -0.177276 0.436648 -0.036459 11.00000 -1.50000
H31C 2 -0.117986 0.527703 -0.022850 11.00000 -1.50000
AFIX 0
C36 1 0.156928 0.240459 0.118688 11.00000 0.03332 0.03316 =
0.02776 0.00683 -0.00159 -0.00822
AFIX 137
H36A 2 0.164774 0.285239 0.090502 11.00000 -1.50000
H36B 2 0.086043 0.227664 0.123907 11.00000 -1.50000
H36C 2 0.191576 0.184498 0.108951 11.00000 -1.50000
AFIX 0
C16 1 0.500912 0.735809 0.143393 11.00000 0.01914 0.03298 =
0.02445 -0.00481 -0.00084 -0.00249
AFIX 137
H16A 2 0.486877 0.714937 0.107516 11.00000 -1.50000
H16B 2 0.565852 0.712642 0.154674 11.00000 -1.50000
H16C 2 0.501756 0.802175 0.144089 11.00000 -1.50000
AFIX 0
C33 1 0.031601 0.693558 0.003230 11.00000 0.01281 0.01882 =
0.02073 0.00015 -0.00203 -0.00067
AFIX 23
H33A 2 0.004478 0.649096 -0.022184 11.00000 -1.20000
H33B 2 0.010960 0.754832 -0.008244 11.00000 -1.20000
AFIX 0
C15 1 0.419642 0.700742 0.180925 11.00000 0.02046 0.02851 =
0.01733 -0.00369 -0.00125 -0.00122
AFIX 13
H15 2 0.432308 0.725611 0.216939 11.00000 -1.20000
AFIX 0
C25 1 -0.278468 0.504718 0.128431 11.00000 0.01655 0.03990 =
0.02948 0.00047 0.00123 -0.00111
AFIX 137
H25A 2 -0.285475 0.457118 0.101787 11.00000 -1.50000
H25B 2 -0.341026 0.538494 0.131275 11.00000 -1.50000
H25C 2 -0.262536 0.477182 0.162521 11.00000 -1.50000
AFIX 0
C18 1 0.299686 0.870455 0.159822 11.00000 0.02065 0.02310 =
0.02819 -0.00521 -0.00026 -0.00093
AFIX 13
H18 2 0.357234 0.887459 0.136890 11.00000 -1.20000
AFIX 0
C38 1 0.368292 0.357808 0.264508 11.00000 0.03250 0.05392 =
0.02796 0.00819 -0.00893 0.00424
AFIX 137
H38A 2 0.331973 0.329042 0.293498 11.00000 -1.50000
H38B 2 0.409238 0.407314 0.278349 11.00000 -1.50000
H38C 2 0.411179 0.312927 0.247372 11.00000 -1.50000
AFIX 0
C17 1 0.425790 0.597567 0.183233 11.00000 0.02145 0.02913 =
0.02883 0.00183 0.00327 0.00499
AFIX 137
H17A 2 0.377241 0.574685 0.208778 11.00000 -1.50000
H17B 2 0.492917 0.579418 0.194024 11.00000 -1.50000
H17C 2 0.411159 0.572363 0.148378 11.00000 -1.50000
AFIX 0
C19 1 0.324648 0.906332 0.214888 11.00000 0.04123 0.03235 =
0.04391 -0.01473 -0.00779 0.00000
AFIX 137
H19A 2 0.269143 0.893677 0.238819 11.00000 -1.50000
H19B 2 0.335857 0.971856 0.213133 11.00000 -1.50000
H19C 2 0.384909 0.876409 0.227927 11.00000 -1.50000
AFIX 0
C32 1 -0.010054 0.674398 0.057779 11.00000 0.01338 0.01438 =
0.02442 -0.00076 0.00244 -0.00010
AFIX 23
H32A 2 0.013335 0.721702 0.082487 11.00000 -1.20000
H32B 2 -0.083623 0.677294 0.056483 11.00000 -1.20000
AFIX 0
C2 1 0.528386 0.388811 -0.001061 11.00000 0.02461 0.02886 =
0.03861 -0.00579 -0.00579 0.01252
AFIX 137
H2A 2 0.503501 0.328199 -0.009680 11.00000 -1.50000
H2B 2 0.573591 0.384964 0.029144 11.00000 -1.50000
H2C 2 0.564180 0.413647 -0.031430 11.00000 -1.50000
AFIX 0
C9 1 0.428101 0.594251 -0.105737 11.00000 0.03143 0.02092 =
0.03900 -0.00192 0.01646 -0.00065
AFIX 137
H9A 2 0.380912 0.634674 -0.088027 11.00000 -1.50000
H9B 2 0.438504 0.614962 -0.141989 11.00000 -1.50000
H9C 2 0.491666 0.594859 -0.086816 11.00000 -1.50000
AFIX 0
C13 1 0.094237 0.733140 0.200767 11.00000 0.02107 0.04136 =
0.02467 -0.00432 0.00289 -0.00144
AFIX 137
H13A 2 0.096842 0.796838 0.211542 11.00000 -1.50000
H13B 2 0.047753 0.700255 0.223546 11.00000 -1.50000
H13C 2 0.071667 0.729175 0.164139 11.00000 -1.50000
AFIX 0
C5 1 0.263087 0.289851 -0.000689 11.00000 0.02734 0.01786 =
0.03378 -0.00039 0.00724 -0.00128
AFIX 137
H5A 2 0.318229 0.287097 0.024521 11.00000 -1.50000
H5B 2 0.239078 0.228424 -0.007946 11.00000 -1.50000
H5C 2 0.208849 0.326128 0.014175 11.00000 -1.50000
AFIX 0
C34 1 0.410524 0.212433 0.149647 11.00000 0.03339 0.03589 =
0.07430 -0.00385 0.00155 0.01128
AFIX 137
H34A 2 0.454934 0.197586 0.179020 11.00000 -1.50000
H34B 2 0.442242 0.195194 0.116370 11.00000 -1.50000
H34C 2 0.347795 0.179266 0.153633 11.00000 -1.50000
AFIX 0
N6 3 0.199068 0.276045 0.167231 11.00000 0.02828 0.02446 =
0.02140 0.00575 -0.00163 -0.00327
C4 1 0.298975 0.333191 -0.051662 11.00000 0.02300 0.01561 =
0.02786 -0.00476 0.00866 -0.00370
AFIX 13
H4 2 0.357810 0.298287 -0.064696 11.00000 -1.20000
AFIX 0
C37 1 0.182707 0.217162 0.212829 11.00000 0.05161 0.03758 =
0.03194 0.01249 0.00150 -0.00973
AFIX 137
H37A 2 0.214477 0.158368 0.206628 11.00000 -1.50000
H37B 2 0.111093 0.208444 0.218100 11.00000 -1.50000
H37C 2 0.211602 0.245268 0.244273 11.00000 -1.50000
AFIX 0
C20 1 0.210557 0.923155 0.138791 11.00000 0.02944 0.02188 =
0.03889 -0.00609 -0.00039 0.00086
AFIX 137
H20A 2 0.196751 0.904340 0.102507 11.00000 -1.50000
H20B 2 0.225387 0.988139 0.139504 11.00000 -1.50000
H20C 2 0.152244 0.910859 0.160843 11.00000 -1.50000
AFIX 0
C27 1 -0.030041 0.481444 0.203240 11.00000 0.02717 0.03140 =
0.01804 0.00337 -0.00429 -0.00102
AFIX 137
H27A 2 0.002576 0.540701 0.201079 11.00000 -1.50000
H27B 2 0.004492 0.443712 0.229208 11.00000 -1.50000
H27C 2 -0.099545 0.489504 0.213960 11.00000 -1.50000
AFIX 0
C7 1 0.386369 0.498037 -0.106328 11.00000 0.01907 0.01972 =
0.02399 -0.00260 0.00122 -0.00060
AFIX 13
H7 2 0.326288 0.500594 -0.129522 11.00000 -1.20000
AFIX 0
C3 1 0.480399 0.543482 0.029142 11.00000 0.02363 0.02599 =
0.03772 -0.00884 -0.01169 0.00078
AFIX 137
H3A 2 0.514887 0.571692 -0.000648 11.00000 -1.50000
H3B 2 0.526886 0.536327 0.058589 11.00000 -1.50000
H3C 2 0.424686 0.581978 0.040071 11.00000 -1.50000
AFIX 0
HKLF 4
REM UDKINQ in P212121 for DMK/STL
REM R1 = 0.0255 for 10604 Fo > 4sig(Fo) and 0.0277 for all 11116 data
REM 494 parameters refined using 0 restraints
END
WGHT 0.0258 0.0000
REM Instructions for potential hydrogen bonds
HTAB C38 N5
HTAB C34 N6
HTAB C37 N7
REM Highest difference peak 1.546, deepest hole -0.401, 1-sigma level 0.084
Q1 1 0.4169 0.5588 0.0721 11.00000 0.05 1.55
Q2 1 0.3054 0.4425 0.2838 11.00000 0.05 1.51
Q3 1 0.1963 0.3325 0.0725 11.00000 0.05 1.49
Q4 1 0.3030 0.6746 0.2824 11.00000 0.05 0.83
Q5 1 0.1785 0.5637 0.1055 11.00000 0.05 0.76
Q6 1 0.2314 0.5608 0.1065 11.00000 0.05 0.72
Q7 1 0.2932 0.5626 0.0725 11.00000 0.05 0.69
Q8 1 0.1559 0.5571 0.0382 11.00000 0.05 0.69
Q9 1 0.2343 0.5594 0.0358 11.00000 0.05 0.65
Q10 1 0.4135 0.3313 0.0739 11.00000 0.05 0.60
Q11 1 0.1383 0.5156 0.0724 11.00000 0.05 0.55
Q12 1 0.0830 0.4407 0.2825 11.00000 0.05 0.52
Q13 1 0.2964 0.3770 0.1938 11.00000 0.05 0.47
Q14 1 0.1441 0.5969 0.0739 11.00000 0.05 0.44
Q15 1 0.1005 0.5531 0.0718 11.00000 0.05 0.40
Q16 1 -0.0046 0.5595 0.0667 11.00000 0.05 0.36
Q17 1 0.2077 0.5421 -0.0272 11.00000 0.05 0.34
Q18 1 0.2000 0.5063 0.1315 11.00000 0.05 0.33
Q19 1 -0.1894 0.6009 0.1372 11.00000 0.05 0.32
Q20 1 0.2180 0.6799 0.2221 11.00000 0.05 0.32
;
_shelx_res_checksum 1435
_olex2_submission_original_sample_id UDKINQ
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.654(4)
2 0.346(4)
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_4
_database_code_depnum_ccdc_archive 'CCDC 1547175'
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_audit_creation_method SHELXL-2014/7
_shelx_SHELXL_version_number 2014/7
_chemical_name_systematic ?
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C66 H150 N8 S2 Si6 U2'
_chemical_formula_sum 'C66 H150 N8 S2 Si6 U2'
_chemical_formula_weight 1764.66
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'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 21/c'
_space_group_name_Hall '-P 2ybc'
_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.
;
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'
_cell_length_a 12.9125(10)
_cell_length_b 22.4587(4)
_cell_length_c 23.3257(18)
_cell_angle_alpha 90
_cell_angle_beta 144.194(17)
_cell_angle_gamma 90
_cell_volume 3957.5(10)
_cell_formula_units_Z 2
_cell_measurement_temperature 120(2)
_cell_measurement_reflns_used 24764
_cell_measurement_theta_min 3.74
_cell_measurement_theta_max 74.41
_exptl_crystal_description block
_exptl_crystal_colour orange
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.481
_exptl_crystal_F_000 1804
_exptl_transmission_factor_min ?
_exptl_transmission_factor_max ?
_exptl_crystal_size_min 0.0830
_exptl_crystal_size_mid 0.1217
_exptl_crystal_size_max 0.1618
_exptl_absorpt_coefficient_mu 13.098
_shelx_estimated_absorpt_T_min ?
_shelx_estimated_absorpt_T_max ?
_exptl_absorpt_correction_type analytical
_exptl_absorpt_correction_T_min 0.261
_exptl_absorpt_correction_T_max 0.479
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_diffrn_ambient_temperature 120(2)
_diffrn_radiation_wavelength 1.54184
_diffrn_radiation_type CuK\a
_diffrn_radiation_source 'SuperNova (Cu) X-ray Source'
_diffrn_measurement_device_type 'SuperNova, Single source at offset, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_detector_area_resol_mean 10.3613
_diffrn_reflns_number 39692
_diffrn_reflns_av_unetI/netI 0.0203
_diffrn_reflns_av_R_equivalents 0.0368
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_h_max 16
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_k_max 27
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_limit_l_max 27
_diffrn_reflns_theta_min 3.790
_diffrn_reflns_theta_max 74.610
_diffrn_reflns_theta_full 67.500
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total 7983
_reflns_number_gt 7879
_reflns_threshold_expression 'I > 2\s(I)'
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_max .
_reflns_Friedel_fraction_full .
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec 3 2012,18:21:49)
;
_computing_structure_solution 'SHELXS97 (Sheldrick, 2008)'
_computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)'
_computing_publication_material
;
enCIFer (Allen et al., 2004); PLATON (Spek, 2009)
;
_refine_special_details ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0289P)^2^+10.1320P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens 'geom, Me from difmap'
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_extinction_coef .
_refine_ls_number_reflns 7983
_refine_ls_number_parameters 397
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0256
_refine_ls_R_factor_gt 0.0251
_refine_ls_wR_factor_ref 0.0619
_refine_ls_wR_factor_gt 0.0616
_refine_ls_goodness_of_fit_ref 1.068
_refine_ls_restrained_S_all 1.068
_refine_ls_shift/su_max 0.003
_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_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
U1 U 0.22776(2) 0.47217(2) 0.80775(2) 0.01526(4) Uani 1 1 d . . . . .
S1 S 0.42822(12) 0.48087(4) 1.00175(6) 0.02744(18) Uani 1 1 d . . . . .
N1 N -0.0332(4) 0.47692(12) 0.7373(2) 0.0182(6) Uani 1 1 d . . . . .
Si1 Si -0.11580(11) 0.46424(4) 0.76952(6) 0.01705(17) Uani 1 1 d . . . . .
C1 C -0.0988(5) 0.53625(15) 0.8190(3) 0.0244(7) Uani 1 1 d . . . . .
H1 H 0.0249 0.5508 0.8683 0.029 Uiso 1 1 calc R U . . .
C2 C -0.1204(5) 0.53134(17) 0.8745(3) 0.0284(8) Uani 1 1 d . . . . .
H2A H -0.2371 0.5147 0.8311 0.043 Uiso 1 1 calc R U . . .
H2B H -0.1098 0.5710 0.8966 0.043 Uiso 1 1 calc R U . . .
H2C H -0.0281 0.5052 0.9315 0.043 Uiso 1 1 calc R U . . .
C3 C -0.2196(5) 0.58533(16) 0.7404(3) 0.0304(8) Uani 1 1 d . . . . .
H3A H -0.1896 0.5925 0.7137 0.046 Uiso 1 1 calc R U . . .
H3B H -0.2028 0.6221 0.7700 0.046 Uiso 1 1 calc R U . . .
H3C H -0.3435 0.5727 0.6877 0.046 Uiso 1 1 calc R U . . .
C4 C -0.3572(4) 0.43876(15) 0.6558(2) 0.0211(7) Uani 1 1 d . . . . .
H4 H -0.4139 0.4649 0.6008 0.025 Uiso 1 1 calc R U . . .
C5 C -0.4675(5) 0.44624(17) 0.6614(3) 0.0258(7) Uani 1 1 d . . . . .
H5A H -0.4132 0.4232 0.7169 0.039 Uiso 1 1 calc R U . . .
H5B H -0.5882 0.4319 0.6005 0.039 Uiso 1 1 calc R U . . .
H5C H -0.4711 0.4884 0.6705 0.039 Uiso 1 1 calc R U . . .
C6 C -0.3767(5) 0.37461(17) 0.6250(3) 0.0297(8) Uani 1 1 d . . . . .
H6A H -0.2970 0.3684 0.6281 0.045 Uiso 1 1 calc R U . . .
H6B H -0.4992 0.3678 0.5578 0.045 Uiso 1 1 calc R U . . .
H6C H -0.3464 0.3467 0.6693 0.045 Uiso 1 1 calc R U . . .
C7 C 0.0238(4) 0.40684(15) 0.8712(2) 0.0220(7) Uani 1 1 d . . . . .
H7 H 0.1294 0.4285 0.9339 0.026 Uiso 1 1 calc R U . . .
C8 C 0.0950(5) 0.35697(15) 0.8652(3) 0.0238(7) Uani 1 1 d . . . . .
H8A H -0.0042 0.3352 0.8035 0.036 Uiso 1 1 calc R U . . .
H8B H 0.1664 0.3296 0.9204 0.036 Uiso 1 1 calc R U . . .
H8C H 0.1686 0.3741 0.8678 0.036 Uiso 1 1 calc R U . . .
C9 C -0.0693(5) 0.37859(17) 0.8816(3) 0.0295(8) Uani 1 1 d . . . . .
H9A H -0.1079 0.4100 0.8906 0.044 Uiso 1 1 calc R U . . .
H9B H 0.0133 0.3520 0.9385 0.044 Uiso 1 1 calc R U . . .
H9C H -0.1724 0.3558 0.8223 0.044 Uiso 1 1 calc R U . . .
C10 C -0.1640(4) 0.50364(16) 0.6383(2) 0.0221(7) Uani 1 1 d . . . . .
H10A H -0.1140 0.5401 0.6432 0.027 Uiso 1 1 calc R U . . .
H10B H -0.2730 0.5147 0.6103 0.027 Uiso 1 1 calc R U . . .
C11 C -0.2074(5) 0.45833(17) 0.5722(2) 0.0252(7) Uani 1 1 d . . . . .
H11A H -0.2513 0.4209 0.5699 0.030 Uiso 1 1 calc R U . . .
H11B H -0.2999 0.4742 0.5048 0.030 Uiso 1 1 calc R U . . .
N2 N 0.2483(4) 0.37753(12) 0.7835(2) 0.0198(6) Uani 1 1 d . . . . .
Si2 Si 0.42022(11) 0.33045(4) 0.84053(6) 0.01825(17) Uani 1 1 d . . . . .
C12 C 0.6285(5) 0.37754(15) 0.9322(3) 0.0248(7) Uani 1 1 d . . . . .
H12 H 0.6470 0.3919 0.9806 0.030 Uiso 1 1 calc R U . . .
C13 C 0.6178(5) 0.43387(16) 0.8898(3) 0.0274(8) Uani 1 1 d . . . . .
H13A H 0.6192 0.4224 0.8499 0.041 Uiso 1 1 calc R U . . .
H13B H 0.7193 0.4596 0.9436 0.041 Uiso 1 1 calc R U . . .
H13C H 0.5079 0.4553 0.8489 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7959(5) 0.34198(19) 0.9916(3) 0.0415(10) Uani 1 1 d . . . . .
H14A H 0.8149 0.3105 1.0286 0.062 Uiso 1 1 calc R U . . .
H14B H 0.8984 0.3687 1.0372 0.062 Uiso 1 1 calc R U . . .
H14C H 0.7810 0.3241 0.9469 0.062 Uiso 1 1 calc R U . . .
C15 C 0.4554(5) 0.27031(16) 0.9132(3) 0.0258(7) Uani 1 1 d . . . . .
H15 H 0.5208 0.2903 0.9745 0.031 Uiso 1 1 calc R U . . .
C16 C 0.2883(6) 0.24469(17) 0.8655(3) 0.0332(8) Uani 1 1 d . . . . .
H16A H 0.2129 0.2773 0.8452 0.050 Uiso 1 1 calc R U . . .
H16B H 0.3211 0.2193 0.9127 0.050 Uiso 1 1 calc R U . . .
H16C H 0.2237 0.2211 0.8081 0.050 Uiso 1 1 calc R U . . .
C17 C 0.5734(6) 0.21756(19) 0.9476(4) 0.0406(10) Uani 1 1 d . . . . .
H17A H 0.5128 0.1946 0.8906 0.061 Uiso 1 1 calc R U . . .
H17B H 0.5965 0.1919 0.9911 0.061 Uiso 1 1 calc R U . . .
H17C H 0.6858 0.2328 0.9830 0.061 Uiso 1 1 calc R U . . .
C18 C 0.3950(5) 0.28961(16) 0.7576(3) 0.0270(7) Uani 1 1 d . . . . .
H18 H 0.5018 0.2634 0.8034 0.032 Uiso 1 1 calc R U . . .
C19 C 0.4065(7) 0.3281(2) 0.7085(3) 0.0401(10) Uani 1 1 d . . . . .
H19A H 0.3097 0.3572 0.6650 0.060 Uiso 1 1 calc R U . . .
H19B H 0.3970 0.3026 0.6703 0.060 Uiso 1 1 calc R U . . .
H19C H 0.5201 0.3491 0.7589 0.060 Uiso 1 1 calc R U . . .
C20 C 0.2384(6) 0.24649(18) 0.6816(3) 0.0330(9) Uani 1 1 d . . . . .
H20A H 0.2302 0.2218 0.7125 0.050 Uiso 1 1 calc R U . . .
H20B H 0.2564 0.2209 0.6561 0.050 Uiso 1 1 calc R U . . .
H20C H 0.1287 0.2692 0.6276 0.050 Uiso 1 1 calc R U . . .
C21 C 0.0684(4) 0.35144(15) 0.6949(2) 0.0239(7) Uani 1 1 d . . . . .
H21A H -0.0004 0.3554 0.7000 0.029 Uiso 1 1 calc R U . . .
H21B H 0.0782 0.3086 0.6900 0.029 Uiso 1 1 calc R U . . .
C22 C -0.0247(5) 0.38394(16) 0.6050(3) 0.0254(7) Uani 1 1 d . . . . .
H22A H 0.0450 0.3808 0.6005 0.030 Uiso 1 1 calc R U . . .
H22B H -0.1429 0.3663 0.5452 0.030 Uiso 1 1 calc R U . . .
N3 N 0.2192(4) 0.53849(12) 0.7307(2) 0.0185(5) Uani 1 1 d . . . . .
Si3 Si 0.24687(12) 0.61491(4) 0.73320(6) 0.02004(17) Uani 1 1 d . . . . .
C23 C 0.2913(5) 0.65011(16) 0.8256(3) 0.0261(7) Uani 1 1 d . . . . .
H23 H 0.4092 0.6348 0.8912 0.031 Uiso 1 1 calc R U . . .
C24 C 0.1606(6) 0.63339(18) 0.8143(3) 0.0343(9) Uani 1 1 d . . . . .
H24A H 0.0411 0.6458 0.7495 0.051 Uiso 1 1 calc R U . . .
H24B H 0.1942 0.6535 0.8651 0.051 Uiso 1 1 calc R U . . .
H24C H 0.1628 0.5902 0.8212 0.051 Uiso 1 1 calc R U . . .
C25 C 0.3107(6) 0.71805(17) 0.8299(3) 0.0376(10) Uani 1 1 d . . . . .
H25A H 0.4001 0.7277 0.8410 0.056 Uiso 1 1 calc R U . . .
H25B H 0.3475 0.7342 0.8835 0.056 Uiso 1 1 calc R U . . .
H25C H 0.1970 0.7356 0.7677 0.056 Uiso 1 1 calc R U . . .
C26 C 0.4417(5) 0.63241(17) 0.7719(3) 0.0264(7) Uani 1 1 d . . . . .
H26 H 0.4478 0.6768 0.7718 0.032 Uiso 1 1 calc R U . . .
C27 C 0.4293(5) 0.6087(2) 0.7046(3) 0.0342(9) Uani 1 1 d . . . . .
H27A H 0.4452 0.5654 0.7118 0.051 Uiso 1 1 calc R U . . .
H27B H 0.5219 0.6271 0.7227 0.051 Uiso 1 1 calc R U . . .
H27C H 0.3129 0.6185 0.6364 0.051 Uiso 1 1 calc R U . . .
C28 C 0.6156(5) 0.6123(2) 0.8763(3) 0.0354(9) Uani 1 1 d . . . . .
H28A H 0.6328 0.6323 0.9210 0.053 Uiso 1 1 calc R U . . .
H28B H 0.7133 0.6226 0.8943 0.053 Uiso 1 1 calc R U . . .
H28C H 0.6131 0.5691 0.8810 0.053 Uiso 1 1 calc R U . . .
C29 C 0.0464(5) 0.64983(16) 0.6053(3) 0.0259(7) Uani 1 1 d . . . . .
H29 H 0.0082 0.6207 0.5581 0.031 Uiso 1 1 calc R U . . .
C30 C -0.1141(5) 0.66010(18) 0.5719(3) 0.0314(8) Uani 1 1 d . . . . .
H30A H -0.1476 0.6225 0.5752 0.047 Uiso 1 1 calc R U . . .
H30B H -0.2133 0.6748 0.5042 0.047 Uiso 1 1 calc R U . . .
H30C H -0.0844 0.6896 0.6147 0.047 Uiso 1 1 calc R U . . .
C31 C 0.0877(6) 0.70834(18) 0.5924(3) 0.0350(9) Uani 1 1 d . . . . .
H31A H 0.1374 0.7371 0.6419 0.053 Uiso 1 1 calc R U . . .
H31B H -0.0215 0.7245 0.5268 0.053 Uiso 1 1 calc R U . . .
H31C H 0.1734 0.7007 0.6002 0.053 Uiso 1 1 calc R U . . .
C32 C 0.1654(5) 0.50726(16) 0.6528(2) 0.0222(7) Uani 1 1 d . . . . .
H32A H 0.2419 0.4720 0.6810 0.027 Uiso 1 1 calc R U . . .
H32B H 0.1793 0.5343 0.6259 0.027 Uiso 1 1 calc R U . . .
C33 C -0.0257(5) 0.48792(17) 0.5722(2) 0.0246(7) Uani 1 1 d . . . . .
H33A H -0.1026 0.5232 0.5433 0.030 Uiso 1 1 calc R U . . .
H33B H -0.0633 0.4674 0.5198 0.030 Uiso 1 1 calc R U . . .
N4 N -0.0428(4) 0.44718(13) 0.6139(2) 0.0212(6) Uani 1 1 d . . . . .
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
U1 0.01340(6) 0.01564(6) 0.01302(6) 0.00038(3) 0.00993(5) -0.00002(3)
S1 0.0219(4) 0.0400(5) 0.0173(4) -0.0043(3) 0.0153(4) -0.0097(3)
N1 0.0137(13) 0.0203(13) 0.0138(12) 0.0022(10) 0.0097(11) 0.0009(10)
Si1 0.0159(4) 0.0161(4) 0.0171(4) 0.0019(3) 0.0130(4) 0.0015(3)
C1 0.0256(18) 0.0222(16) 0.0277(17) -0.0037(13) 0.0220(16) -0.0023(13)
C2 0.0269(19) 0.032(2) 0.0304(19) -0.0082(14) 0.0240(17) -0.0052(14)
C3 0.038(2) 0.0204(17) 0.042(2) 0.0039(15) 0.0347(19) 0.0061(15)
C4 0.0193(15) 0.0203(15) 0.0194(15) 0.0008(12) 0.0147(14) -0.0001(12)
C5 0.0201(16) 0.0304(18) 0.0271(17) 0.0016(14) 0.0192(15) 0.0007(14)
C6 0.0293(18) 0.0271(18) 0.0340(19) -0.0100(15) 0.0259(17) -0.0083(15)
C7 0.0199(15) 0.0228(16) 0.0185(15) 0.0041(12) 0.0146(14) 0.0024(13)
C8 0.0254(17) 0.0212(16) 0.0250(16) 0.0049(13) 0.0204(15) 0.0037(13)
C9 0.0307(18) 0.0311(19) 0.0323(18) 0.0090(15) 0.0267(17) 0.0060(15)
C10 0.0145(14) 0.0259(17) 0.0184(15) 0.0074(13) 0.0117(13) 0.0040(13)
C11 0.0210(16) 0.0311(17) 0.0183(15) 0.0031(14) 0.0148(14) 0.0012(14)
N2 0.0192(13) 0.0154(12) 0.0185(12) -0.0026(10) 0.0139(12) -0.0024(10)
Si2 0.0206(4) 0.0164(4) 0.0194(4) -0.0005(3) 0.0166(4) -0.0008(3)
C12 0.0218(16) 0.0202(16) 0.0258(16) -0.0009(13) 0.0179(15) -0.0008(13)
C13 0.0265(17) 0.0249(17) 0.0314(18) -0.0037(14) 0.0236(16) -0.0060(14)
C14 0.0227(19) 0.030(2) 0.046(2) -0.0024(18) 0.0227(19) -0.0012(16)
C15 0.0325(18) 0.0209(16) 0.0306(18) 0.0057(14) 0.0269(17) 0.0046(14)
C16 0.044(2) 0.0241(18) 0.049(2) 0.0087(16) 0.042(2) 0.0052(16)
C17 0.040(2) 0.033(2) 0.053(3) 0.0215(19) 0.038(2) 0.0160(18)
C18 0.0335(19) 0.0244(17) 0.0284(17) -0.0035(14) 0.0263(17) -0.0020(15)
C19 0.059(3) 0.040(2) 0.048(2) -0.0081(19) 0.048(2) -0.011(2)
C20 0.043(2) 0.0291(19) 0.0327(19) -0.0093(15) 0.0322(19) -0.0086(17)
C21 0.0223(16) 0.0211(16) 0.0245(16) -0.0049(13) 0.0181(15) -0.0054(13)
C22 0.0221(16) 0.0245(17) 0.0226(16) -0.0069(13) 0.0167(15) -0.0073(13)
N3 0.0194(13) 0.0180(12) 0.0171(12) 0.0011(10) 0.0146(12) -0.0007(10)
Si3 0.0195(4) 0.0181(4) 0.0216(4) 0.0017(3) 0.0165(4) 0.0000(3)
C23 0.0317(18) 0.0212(16) 0.0212(16) -0.0005(13) 0.0206(15) -0.0001(14)
C24 0.042(2) 0.033(2) 0.0317(19) 0.0000(16) 0.0306(19) 0.0039(17)
C25 0.060(3) 0.0241(19) 0.039(2) -0.0033(16) 0.043(2) -0.0034(18)
C26 0.0251(17) 0.0265(17) 0.0285(17) 0.0018(14) 0.0219(16) -0.0009(14)
C27 0.034(2) 0.045(2) 0.037(2) -0.0020(17) 0.0318(19) -0.0039(17)
C28 0.0273(19) 0.044(2) 0.0310(19) 0.0065(17) 0.0229(18) 0.0031(17)
C29 0.0282(18) 0.0241(17) 0.0238(16) 0.0056(13) 0.0208(16) 0.0047(14)
C30 0.0236(17) 0.035(2) 0.0252(17) 0.0099(15) 0.0175(16) 0.0072(15)
C31 0.038(2) 0.031(2) 0.034(2) 0.0118(16) 0.0291(19) 0.0059(17)
C32 0.0236(16) 0.0230(16) 0.0216(15) 0.0015(13) 0.0187(15) 0.0003(13)
C33 0.0272(18) 0.0264(17) 0.0179(15) -0.0010(13) 0.0178(15) -0.0043(14)
N4 0.0218(13) 0.0213(14) 0.0190(13) 0.0008(11) 0.0162(12) -0.0023(11)
_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
U1 N1 2.254(3) . ?
U1 N3 2.268(3) . ?
U1 N2 2.270(3) . ?
U1 N4 2.709(3) . ?
U1 S1 2.8666(12) . ?
U1 S1 2.9280(15) 3_667 ?
S1 S1 2.1041(18) 3_667 ?
S1 U1 2.9281(15) 3_667 ?
N1 C10 1.490(4) . ?
N1 Si1 1.757(3) . ?
Si1 C1 1.893(4) . ?
Si1 C7 1.898(3) . ?
Si1 C4 1.915(4) . ?
C1 C2 1.534(5) . ?
C1 C3 1.540(5) . ?
C1 H1 1.0000 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 C6 1.537(5) . ?
C4 C5 1.543(5) . ?
C4 H4 1.0000 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 C8 1.526(5) . ?
C7 C9 1.542(5) . ?
C7 H7 1.0000 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.524(5) . ?
C10 H10A 0.9900 . ?
C10 H10B 0.9900 . ?
C11 N4 1.473(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
N2 C21 1.491(4) . ?
N2 Si2 1.739(3) . ?
Si2 C12 1.896(4) . ?
Si2 C15 1.912(4) . ?
Si2 C18 1.915(4) . ?
C12 C14 1.540(5) . ?
C12 C13 1.541(5) . ?
C12 H12 1.0000 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C16 1.526(5) . ?
C15 C17 1.544(5) . ?
C15 H15 1.0000 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.535(5) . ?
C18 C19 1.535(5) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 C22 1.512(5) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 N4 1.481(4) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
N3 C32 1.491(4) . ?
N3 Si3 1.744(3) . ?
Si3 C23 1.897(4) . ?
Si3 C26 1.900(4) . ?
Si3 C29 1.921(4) . ?
C23 C24 1.528(6) . ?
C23 C25 1.537(5) . ?
C23 H23 1.0000 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.519(5) . ?
C26 C27 1.539(5) . ?
C26 H26 1.0000 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 C30 1.528(5) . ?
C29 C31 1.537(5) . ?
C29 H29 1.0000 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.512(5) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 N4 1.478(4) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
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
N1 U1 N3 107.93(10) . . ?
N1 U1 N2 105.69(10) . . ?
N3 U1 N2 110.95(10) . . ?
N1 U1 N4 69.57(10) . . ?
N3 U1 N4 69.23(9) . . ?
N2 U1 N4 69.10(9) . . ?
N1 U1 S1 92.86(8) . . ?
N3 U1 S1 127.44(7) . . ?
N2 U1 S1 108.61(7) . . ?
N4 U1 S1 160.01(6) . . ?
N1 U1 S1 128.34(8) . 3_667 ?
N3 U1 S1 90.29(7) . 3_667 ?
N2 U1 S1 112.05(7) . 3_667 ?
N4 U1 S1 157.39(6) . 3_667 ?
S1 U1 S1 42.57(4) . 3_667 ?
S1 S1 U1 70.27(5) 3_667 . ?
S1 S1 U1 67.16(4) 3_667 3_667 ?
U1 S1 U1 137.43(4) . 3_667 ?
C10 N1 Si1 114.2(2) . . ?
C10 N1 U1 107.1(2) . . ?
Si1 N1 U1 138.39(15) . . ?
N1 Si1 C1 108.20(15) . . ?
N1 Si1 C7 110.75(14) . . ?
C1 Si1 C7 107.15(16) . . ?
N1 Si1 C4 109.04(15) . . ?
C1 Si1 C4 110.71(16) . . ?
C7 Si1 C4 110.95(15) . . ?
C2 C1 C3 110.7(3) . . ?
C2 C1 Si1 116.3(2) . . ?
C3 C1 Si1 112.4(3) . . ?
C2 C1 H1 105.5 . . ?
C3 C1 H1 105.5 . . ?
Si1 C1 H1 105.5 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C6 C4 C5 109.2(3) . . ?
C6 C4 Si1 113.2(2) . . ?
C5 C4 Si1 115.3(2) . . ?
C6 C4 H4 106.2 . . ?
C5 C4 H4 106.2 . . ?
Si1 C4 H4 106.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
H5A C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C8 C7 C9 108.5(3) . . ?
C8 C7 Si1 114.5(2) . . ?
C9 C7 Si1 113.9(2) . . ?
C8 C7 H7 106.4 . . ?
C9 C7 H7 106.4 . . ?
Si1 C7 H7 106.4 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
N1 C10 C11 108.9(3) . . ?
N1 C10 U1 45.02(15) . . ?
C11 C10 U1 91.1(2) . . ?
N1 C10 H10A 109.9 . . ?
C11 C10 H10A 109.9 . . ?
U1 C10 H10A 78.5 . . ?
N1 C10 H10B 109.9 . . ?
C11 C10 H10B 109.9 . . ?
U1 C10 H10B 153.0 . . ?
H10A C10 H10B 108.3 . . ?
N4 C11 C10 107.1(3) . . ?
N4 C11 H11A 110.3 . . ?
C10 C11 H11A 110.3 . . ?
N4 C11 H11B 110.3 . . ?
C10 C11 H11B 110.3 . . ?
H11A C11 H11B 108.5 . . ?
C21 N2 Si2 114.1(2) . . ?
C21 N2 U1 110.3(2) . . ?
Si2 N2 U1 135.50(15) . . ?
N2 Si2 C12 106.66(15) . . ?
N2 Si2 C15 110.24(15) . . ?
C12 Si2 C15 107.14(17) . . ?
N2 Si2 C18 116.88(16) . . ?
C12 Si2 C18 109.24(17) . . ?
C15 Si2 C18 106.32(16) . . ?
C14 C12 C13 109.5(3) . . ?
C14 C12 Si2 113.4(3) . . ?
C13 C12 Si2 115.3(2) . . ?
C14 C12 H12 105.9 . . ?
C13 C12 H12 105.9 . . ?
Si2 C12 H12 105.9 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C16 C15 C17 107.8(3) . . ?
C16 C15 Si2 116.2(3) . . ?
C17 C15 Si2 115.3(3) . . ?
C16 C15 H15 105.5 . . ?
C17 C15 H15 105.5 . . ?
Si2 C15 H15 105.5 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 C19 109.1(3) . . ?
C20 C18 Si2 117.1(3) . . ?
C19 C18 Si2 116.3(3) . . ?
C20 C18 H18 104.2 . . ?
C19 C18 H18 104.2 . . ?
Si2 C18 H18 104.2 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
N2 C21 C22 108.9(3) . . ?
N2 C21 H21A 109.9 . . ?
C22 C21 H21A 109.9 . . ?
N2 C21 H21B 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
N4 C22 C21 107.8(3) . . ?
N4 C22 H22A 110.1 . . ?
C21 C22 H22A 110.1 . . ?
N4 C22 H22B 110.1 . . ?
C21 C22 H22B 110.1 . . ?
H22A C22 H22B 108.5 . . ?
C32 N3 Si3 112.6(2) . . ?
C32 N3 U1 109.3(2) . . ?
Si3 N3 U1 137.94(16) . . ?
N3 Si3 C23 108.28(15) . . ?
N3 Si3 C26 112.04(16) . . ?
C23 Si3 C26 108.06(17) . . ?
N3 Si3 C29 111.59(15) . . ?
C23 Si3 C29 112.31(17) . . ?
C26 Si3 C29 104.52(17) . . ?
C24 C23 C25 110.8(3) . . ?
C24 C23 Si3 115.3(3) . . ?
C25 C23 Si3 111.7(3) . . ?
C24 C23 H23 106.1 . . ?
C25 C23 H23 106.1 . . ?
Si3 C23 H23 106.1 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C27 109.1(3) . . ?
C28 C26 Si3 111.5(3) . . ?
C27 C26 Si3 116.2(3) . . ?
C28 C26 H26 106.5 . . ?
C27 C26 H26 106.5 . . ?
Si3 C26 H26 106.5 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C30 C29 C31 108.3(3) . . ?
C30 C29 Si3 114.6(3) . . ?
C31 C29 Si3 114.1(3) . . ?
C30 C29 H29 106.4 . . ?
C31 C29 H29 106.4 . . ?
Si3 C29 H29 106.4 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 C33 109.2(3) . . ?
N3 C32 H32A 109.8 . . ?
C33 C32 H32A 109.8 . . ?
N3 C32 H32B 109.8 . . ?
C33 C32 H32B 109.8 . . ?
H32A C32 H32B 108.3 . . ?
N4 C33 C32 108.8(3) . . ?
N4 C33 H33A 109.9 . . ?
C32 C33 H33A 109.9 . . ?
N4 C33 H33B 109.9 . . ?
C32 C33 H33B 109.9 . . ?
H33A C33 H33B 108.3 . . ?
C11 N4 C33 111.4(3) . . ?
C11 N4 C22 112.2(3) . . ?
C33 N4 C22 112.1(3) . . ?
C11 N4 U1 106.5(2) . . ?
C33 N4 U1 106.97(19) . . ?
C22 N4 U1 107.23(19) . . ?
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
C10 N1 Si1 C1 -83.2(3) . . . . ?
U1 N1 Si1 C1 89.7(2) . . . . ?
C10 N1 Si1 C7 159.6(2) . . . . ?
U1 N1 Si1 C7 -27.5(3) . . . . ?
C10 N1 Si1 C4 37.2(3) . . . . ?
U1 N1 Si1 C4 -149.8(2) . . . . ?
N1 Si1 C1 C2 -165.4(3) . . . . ?
C7 Si1 C1 C2 -45.9(3) . . . . ?
C4 Si1 C1 C2 75.2(3) . . . . ?
N1 Si1 C1 C3 65.5(3) . . . . ?
C7 Si1 C1 C3 -175.0(3) . . . . ?
C4 Si1 C1 C3 -53.9(3) . . . . ?
N1 Si1 C7 C8 -36.0(3) . . . . ?
C1 Si1 C7 C8 -153.8(3) . . . . ?
C4 Si1 C7 C8 85.2(3) . . . . ?
N1 Si1 C7 C9 -161.7(2) . . . . ?
C1 Si1 C7 C9 80.5(3) . . . . ?
C4 Si1 C7 C9 -40.4(3) . . . . ?
Si1 N1 C10 C11 -113.1(3) . . . . ?
U1 N1 C10 C11 71.8(3) . . . . ?
Si1 N1 C10 U1 175.1(3) . . . . ?
N1 C10 C11 N4 -63.6(3) . . . . ?
U1 C10 C11 N4 -21.4(2) . . . . ?
C21 N2 Si2 C12 168.1(2) . . . . ?
U1 N2 Si2 C12 -9.6(3) . . . . ?
C21 N2 Si2 C15 -75.9(3) . . . . ?
U1 N2 Si2 C15 106.4(2) . . . . ?
C21 N2 Si2 C18 45.6(3) . . . . ?
U1 N2 Si2 C18 -132.1(2) . . . . ?
N2 Si2 C12 C14 178.5(3) . . . . ?
C15 Si2 C12 C14 60.4(3) . . . . ?
C18 Si2 C12 C14 -54.3(3) . . . . ?
N2 Si2 C12 C13 -54.1(3) . . . . ?
C15 Si2 C12 C13 -172.2(3) . . . . ?
C18 Si2 C12 C13 73.0(3) . . . . ?
Si2 N2 C21 C22 -110.9(3) . . . . ?
U1 N2 C21 C22 67.4(3) . . . . ?
N2 C21 C22 N4 -61.9(4) . . . . ?
C32 N3 Si3 C23 174.2(2) . . . . ?
U1 N3 Si3 C23 -1.7(3) . . . . ?
C32 N3 Si3 C26 -66.7(3) . . . . ?
U1 N3 Si3 C26 117.4(2) . . . . ?
C32 N3 Si3 C29 50.1(3) . . . . ?
U1 N3 Si3 C29 -125.8(2) . . . . ?
N3 Si3 C23 C24 -50.2(3) . . . . ?
C26 Si3 C23 C24 -171.8(3) . . . . ?
C29 Si3 C23 C24 73.4(3) . . . . ?
N3 Si3 C23 C25 -177.9(3) . . . . ?
C26 Si3 C23 C25 60.5(3) . . . . ?
C29 Si3 C23 C25 -54.3(3) . . . . ?
Si3 N3 C32 C33 -108.8(3) . . . . ?
U1 N3 C32 C33 68.3(3) . . . . ?
N3 C32 C33 N4 -60.1(4) . . . . ?
C10 C11 N4 C33 -91.1(3) . . . . ?
C10 C11 N4 C22 142.3(3) . . . . ?
C10 C11 N4 U1 25.3(3) . . . . ?
C32 C33 N4 C11 140.4(3) . . . . ?
C32 C33 N4 C22 -92.9(3) . . . . ?
C32 C33 N4 U1 24.3(3) . . . . ?
C21 C22 N4 C11 -88.8(3) . . . . ?
C21 C22 N4 C33 144.9(3) . . . . ?
C21 C22 N4 U1 27.8(3) . . . . ?
_refine_diff_density_max 1.142
_refine_diff_density_min -1.949
_refine_diff_density_rms 0.099
_shelx_res_file
;
ubmgmx.res created by SHELXL-2014/7
TITL ubmgmx in P21/c #14
REM reset to P21/c #14
CELL 1.54184 12.912494 22.45872 23.325674 90 144.1938 90
ZERR 4 0.000973 0.000366 0.00176 0 0.017 0
LATT 1
SYMM -X,0.5+Y,0.5-Z
SFAC C H N S Si U
UNIT 132 300 16 4 12 4
L.S. 16
PLAN 20
TEMP -153(2)
CONN 6 U1
BOND $h
fmap 2
acta 135
MORE -1
CONF
OMIT -10 1 27
OMIT 1 27 0
OMIT -5 0 6
REM
REM
REM
WGHT 0.028900 10.132000
FVAR 2.11805
U1 6 0.227765 0.472168 0.807750 11.00000 0.01340 0.01564 =
0.01302 0.00038 0.00993 -0.00002
S1 4 0.428218 0.480874 1.001754 11.00000 0.02195 0.03997 =
0.01728 -0.00431 0.01525 -0.00969
N1 3 -0.033172 0.476915 0.737283 11.00000 0.01371 0.02033 =
0.01382 0.00216 0.00973 0.00086
SI1 5 -0.115795 0.464244 0.769516 11.00000 0.01591 0.01612 =
0.01710 0.00189 0.01296 0.00147
C1 1 -0.098793 0.536246 0.819019 11.00000 0.02557 0.02215 =
0.02767 -0.00369 0.02203 -0.00233
AFIX 13
H1 2 0.024861 0.550764 0.868306 11.00000 -1.20000
AFIX 0
C2 1 -0.120413 0.531339 0.874546 11.00000 0.02686 0.03162 =
0.03043 -0.00816 0.02402 -0.00523
AFIX 137
H2A 2 -0.237125 0.514684 0.831052 11.00000 -1.50000
H2B 2 -0.109777 0.570963 0.896576 11.00000 -1.50000
H2C 2 -0.028147 0.505234 0.931478 11.00000 -1.50000
AFIX 0
C3 1 -0.219645 0.585331 0.740432 11.00000 0.03847 0.02037 =
0.04209 0.00387 0.03471 0.00607
AFIX 137
H3A 2 -0.189557 0.592490 0.713658 11.00000 -1.50000
H3B 2 -0.202822 0.622086 0.769965 11.00000 -1.50000
H3C 2 -0.343474 0.572658 0.687656 11.00000 -1.50000
AFIX 0
C4 1 -0.357168 0.438764 0.655762 11.00000 0.01930 0.02031 =
0.01937 0.00082 0.01474 -0.00007
AFIX 13
H4 2 -0.413942 0.464857 0.600801 11.00000 -1.20000
AFIX 0
C5 1 -0.467464 0.446236 0.661443 11.00000 0.02014 0.03039 =
0.02706 0.00161 0.01918 0.00066
AFIX 137
H5A 2 -0.413192 0.423192 0.716856 11.00000 -1.50000
H5B 2 -0.588175 0.431855 0.600536 11.00000 -1.50000
H5C 2 -0.471086 0.488407 0.670546 11.00000 -1.50000
AFIX 0
C6 1 -0.376718 0.374614 0.624959 11.00000 0.02931 0.02712 =
0.03403 -0.00996 0.02594 -0.00827
AFIX 137
H6A 2 -0.297004 0.368428 0.628140 11.00000 -1.50000
H6B 2 -0.499228 0.367834 0.557780 11.00000 -1.50000
H6C 2 -0.346390 0.346670 0.669312 11.00000 -1.50000
AFIX 0
C7 1 0.023820 0.406838 0.871241 11.00000 0.01987 0.02278 =
0.01850 0.00409 0.01456 0.00235
AFIX 13
H7 2 0.129394 0.428524 0.933900 11.00000 -1.20000
AFIX 0
C8 1 0.095017 0.356969 0.865196 11.00000 0.02539 0.02116 =
0.02497 0.00491 0.02044 0.00367
AFIX 137
H8A 2 -0.004201 0.335214 0.803510 11.00000 -1.50000
H8B 2 0.166381 0.329616 0.920416 11.00000 -1.50000
H8C 2 0.168582 0.374059 0.867780 11.00000 -1.50000
AFIX 0
C9 1 -0.069279 0.378586 0.881626 11.00000 0.03069 0.03106 =
0.03228 0.00899 0.02668 0.00600
AFIX 137
H9A 2 -0.107867 0.410033 0.890611 11.00000 -1.50000
H9B 2 0.013278 0.351966 0.938524 11.00000 -1.50000
H9C 2 -0.172402 0.355805 0.822343 11.00000 -1.50000
AFIX 0
C10 1 -0.163951 0.503637 0.638274 11.00000 0.01446 0.02585 =
0.01842 0.00737 0.01172 0.00403
AFIX 23
H10A 2 -0.113985 0.540112 0.643210 11.00000 -1.20000
H10B 2 -0.273017 0.514666 0.610306 11.00000 -1.20000
AFIX 0
C11 1 -0.207376 0.458335 0.572199 11.00000 0.02097 0.03112 =
0.01829 0.00308 0.01484 0.00122
AFIX 23
H11A 2 -0.251287 0.420927 0.569859 11.00000 -1.20000
H11B 2 -0.299935 0.474181 0.504761 11.00000 -1.20000
AFIX 0
N2 3 0.248304 0.377529 0.783463 11.00000 0.01915 0.01541 =
0.01849 -0.00262 0.01393 -0.00238
SI2 5 0.420222 0.330448 0.840535 11.00000 0.02063 0.01642 =
0.01943 -0.00046 0.01661 -0.00082
C12 1 0.628458 0.377538 0.932150 11.00000 0.02184 0.02016 =
0.02578 -0.00095 0.01792 -0.00079
AFIX 13
H12 2 0.647020 0.391905 0.980614 11.00000 -1.20000
AFIX 0
C13 1 0.617755 0.433868 0.889777 11.00000 0.02650 0.02491 =
0.03140 -0.00374 0.02362 -0.00602
AFIX 137
H13A 2 0.619215 0.422448 0.849886 11.00000 -1.50000
H13B 2 0.719347 0.459644 0.943552 11.00000 -1.50000
H13C 2 0.507896 0.455333 0.848948 11.00000 -1.50000
AFIX 0
C14 1 0.795903 0.341980 0.991622 11.00000 0.02274 0.03014 =
0.04630 -0.00238 0.02265 -0.00120
AFIX 137
H14A 2 0.814881 0.310496 1.028575 11.00000 -1.50000
H14B 2 0.898389 0.368729 1.037222 11.00000 -1.50000
H14C 2 0.780985 0.324090 0.946910 11.00000 -1.50000
AFIX 0
C15 1 0.455384 0.270309 0.913220 11.00000 0.03246 0.02092 =
0.03061 0.00567 0.02695 0.00457
AFIX 13
H15 2 0.520843 0.290317 0.974505 11.00000 -1.20000
AFIX 0
C16 1 0.288319 0.244687 0.865529 11.00000 0.04396 0.02410 =
0.04923 0.00873 0.04152 0.00524
AFIX 137
H16A 2 0.212923 0.277293 0.845218 11.00000 -1.50000
H16B 2 0.321074 0.219257 0.912687 11.00000 -1.50000
H16C 2 0.223699 0.221059 0.808064 11.00000 -1.50000
AFIX 0
C17 1 0.573379 0.217564 0.947641 11.00000 0.03961 0.03303 =
0.05301 0.02149 0.03837 0.01601
AFIX 137
H17A 2 0.512790 0.194590 0.890593 11.00000 -1.50000
H17B 2 0.596468 0.191876 0.991136 11.00000 -1.50000
H17C 2 0.685753 0.232756 0.983037 11.00000 -1.50000
AFIX 0
C18 1 0.395023 0.289610 0.757604 11.00000 0.03354 0.02439 =
0.02844 -0.00354 0.02627 -0.00204
AFIX 13
H18 2 0.501773 0.263374 0.803396 11.00000 -1.20000
AFIX 0
C19 1 0.406480 0.328110 0.708498 11.00000 0.05850 0.03979 =
0.04753 -0.00811 0.04838 -0.01053
AFIX 137
H19A 2 0.309659 0.357151 0.665004 11.00000 -1.50000
H19B 2 0.396951 0.302627 0.670255 11.00000 -1.50000
H19C 2 0.520145 0.349130 0.758887 11.00000 -1.50000
AFIX 0
C20 1 0.238429 0.246486 0.681562 11.00000 0.04342 0.02914 =
0.03268 -0.00928 0.03215 -0.00857
AFIX 137
H20A 2 0.230240 0.221839 0.712454 11.00000 -1.50000
H20B 2 0.256396 0.220865 0.656120 11.00000 -1.50000
H20C 2 0.128657 0.269215 0.627555 11.00000 -1.50000
AFIX 0
C21 1 0.068385 0.351443 0.694928 11.00000 0.02227 0.02115 =
0.02447 -0.00487 0.01815 -0.00538
AFIX 23
H21A 2 -0.000411 0.355418 0.699963 11.00000 -1.20000
H21B 2 0.078237 0.308579 0.689975 11.00000 -1.20000
AFIX 0
C22 1 -0.024736 0.383941 0.605009 11.00000 0.02208 0.02447 =
0.02262 -0.00685 0.01665 -0.00730
AFIX 23
H22A 2 0.044957 0.380785 0.600484 11.00000 -1.20000
H22B 2 -0.142946 0.366257 0.545174 11.00000 -1.20000
AFIX 0
N3 3 0.219204 0.538494 0.730653 11.00000 0.01936 0.01799 =
0.01711 0.00109 0.01457 -0.00073
SI3 5 0.246867 0.614908 0.733200 11.00000 0.01945 0.01811 =
0.02161 0.00168 0.01645 0.00001
C23 1 0.291253 0.650110 0.825619 11.00000 0.03171 0.02121 =
0.02125 -0.00048 0.02061 -0.00005
AFIX 13
H23 2 0.409205 0.634764 0.891235 11.00000 -1.20000
AFIX 0
C24 1 0.160645 0.633388 0.814337 11.00000 0.04180 0.03335 =
0.03168 0.00004 0.03062 0.00390
AFIX 137
H24A 2 0.041109 0.645762 0.749514 11.00000 -1.50000
H24B 2 0.194224 0.653493 0.865081 11.00000 -1.50000
H24C 2 0.162832 0.590186 0.821182 11.00000 -1.50000
AFIX 0
C25 1 0.310716 0.718051 0.829861 11.00000 0.06028 0.02408 =
0.03923 -0.00333 0.04261 -0.00338
AFIX 137
H25A 2 0.400132 0.727730 0.841027 11.00000 -1.50000
H25B 2 0.347462 0.734161 0.883545 11.00000 -1.50000
H25C 2 0.196967 0.735593 0.767715 11.00000 -1.50000
AFIX 0
C26 1 0.441652 0.632413 0.771929 11.00000 0.02512 0.02649 =
0.02854 0.00177 0.02195 -0.00093
AFIX 13
H26 2 0.447835 0.676785 0.771757 11.00000 -1.20000
AFIX 0
C27 1 0.429290 0.608684 0.704596 11.00000 0.03407 0.04462 =
0.03747 -0.00195 0.03185 -0.00389
AFIX 137
H27A 2 0.445154 0.565377 0.711845 11.00000 -1.50000
H27B 2 0.521930 0.627105 0.722725 11.00000 -1.50000
H27C 2 0.312917 0.618466 0.636351 11.00000 -1.50000
AFIX 0
C28 1 0.615637 0.612317 0.876322 11.00000 0.02735 0.04408 =
0.03100 0.00647 0.02286 0.00310
AFIX 137
H28A 2 0.632771 0.632274 0.920962 11.00000 -1.50000
H28B 2 0.713294 0.622598 0.894341 11.00000 -1.50000
H28C 2 0.613102 0.569112 0.881016 11.00000 -1.50000
AFIX 0
C29 1 0.046375 0.649831 0.605283 11.00000 0.02824 0.02414 =
0.02377 0.00562 0.02076 0.00470
AFIX 13
H29 2 0.008231 0.620750 0.558135 11.00000 -1.20000
AFIX 0
C30 1 -0.114121 0.660096 0.571858 11.00000 0.02357 0.03454 =
0.02524 0.00987 0.01750 0.00719
AFIX 137
H30A 2 -0.147619 0.622526 0.575227 11.00000 -1.50000
H30B 2 -0.213303 0.674790 0.504239 11.00000 -1.50000
H30C 2 -0.084371 0.689557 0.614672 11.00000 -1.50000
AFIX 0
C31 1 0.087682 0.708344 0.592390 11.00000 0.03848 0.03086 =
0.03416 0.01184 0.02911 0.00589
AFIX 137
H31A 2 0.137426 0.737123 0.641885 11.00000 -1.50000
H31B 2 -0.021479 0.724484 0.526836 11.00000 -1.50000
H31C 2 0.173438 0.700736 0.600229 11.00000 -1.50000
AFIX 0
C32 1 0.165394 0.507257 0.652841 11.00000 0.02358 0.02298 =
0.02163 0.00147 0.01868 0.00029
AFIX 23
H32A 2 0.241881 0.472049 0.680974 11.00000 -1.20000
H32B 2 0.179300 0.534294 0.625866 11.00000 -1.20000
AFIX 0
C33 1 -0.025726 0.487920 0.572172 11.00000 0.02723 0.02642 =
0.01785 -0.00096 0.01779 -0.00429
AFIX 23
H33A 2 -0.102566 0.523152 0.543272 11.00000 -1.20000
H33B 2 -0.063263 0.467416 0.519769 11.00000 -1.20000
AFIX 0
N4 3 -0.042825 0.447182 0.613936 11.00000 0.02181 0.02125 =
0.01901 0.00077 0.01624 -0.00229
HKLF 4
REM ubmgmx in P21/c #14
REM R1 = 0.0251 for 7879 Fo > 4sig(Fo) and 0.0256 for all 7983 data
REM 397 parameters refined using 0 restraints
END
WGHT 0.0289 10.1489
REM Highest difference peak 1.142, deepest hole -1.949, 1-sigma level 0.099
Q1 1 0.2662 0.6232 0.7771 11.00000 0.05 1.14
Q2 1 0.2780 0.4803 0.8622 11.00000 0.05 1.07
Q3 1 0.1976 0.4714 0.8216 11.00000 0.05 1.04
Q4 1 0.2989 0.4732 0.7872 11.00000 0.05 1.02
Q5 1 0.3144 0.4946 0.8419 11.00000 0.05 0.98
Q6 1 0.3173 0.4585 0.8405 11.00000 0.05 0.88
Q7 1 0.1275 0.4720 0.8254 11.00000 0.05 0.86
Q8 1 0.3719 0.3983 0.9795 11.00000 0.05 0.82
Q9 1 0.0719 0.4735 0.7114 11.00000 0.05 0.74
Q10 1 0.1220 0.4481 0.7780 11.00000 0.05 0.74
Q11 1 0.1282 0.4981 0.7838 11.00000 0.05 0.71
Q12 1 0.2293 0.5208 0.8544 11.00000 0.05 0.68
Q13 1 0.4979 0.6306 0.8391 11.00000 0.05 0.65
Q14 1 0.2488 0.4189 0.8181 11.00000 0.05 0.64
Q15 1 0.5615 0.6943 0.8618 11.00000 0.05 0.63
Q16 1 0.2419 0.5231 0.7664 11.00000 0.05 0.63
Q17 1 0.2401 0.4397 0.8643 11.00000 0.05 0.59
Q18 1 0.4120 0.4715 0.9173 11.00000 0.05 0.57
Q19 1 0.0693 0.5230 0.7947 11.00000 0.05 0.53
Q20 1 0.0983 0.4234 0.6859 11.00000 0.05 0.53
;
_shelx_res_checksum 93341
#######################################################################
#
# This file contains crystal structure data downloaded from the
# Cambridge Structural Database (CSD) hosted by the Cambridge
# Crystallographic Data Centre (CCDC).
#
# Full information about CCDC data access policies and citation
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1
#
# Audit and citation data items may have been added by the CCDC.
# Please retain this information to preserve the provenance of
# this file and to allow appropriate attribution of the data.
#
#######################################################################
data_6
_database_code_depnum_ccdc_archive 'CCDC 1547177'
_audit_update_record
;
2017-04-30 deposited with the CCDC.
2017-07-05 downloaded from the CCDC.
;
_refine_special_details
;
Each triisopropyl silyl group is disordered over two orientations.
In each case the occupancies were allowed to freely refine, converging at final ratios of 0.50:0.50, 0.52:0.48 and 0.55:0.45.
Chemically equivalent 1,2 N-Si, Si-C and C-C distances within all triisopropyl silyl groups were restrained to be approximately equal.
Enhanced rigid bond, and similarity thermal restraints were applied to disordered components to aid refinement.
;
_vrf_PLAT971_6
;
PROBLEM: Check Calcd Residual Density 0.81A From U1 6.30 eA-3
RESPONSE: Residual density is close to Uranium and present
despite applying the correct absorption correction.
It is not chemically significant.
;
_vrf_PLAT973_6
;
PROBLEM: Check Calcd Positive Residual Density on U1 2.58 eA-3
RESPONSE: Residual density is close to Uranium and present
despite applying the correct absorption correction.
It is not chemically significant.
;
_audit_creation_date 2017-04-27
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_shelx_SHELXL_version_number 2016/6
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C66 H150 N8 Si6 Te U2'
_chemical_formula_sum 'C66 H150 N8 Si6 Te U2'
_chemical_formula_weight 1828.13
_chemical_melting_point ?
_chemical_oxdiff_formula 'C66 H150 N8 Si6 Te U2'
_chemical_oxdiff_usercomment
'UBMGNF #12563 for BMG/STL in fomblin oil on micromount'
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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Te Te -0.1759 6.3531 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
U U -4.3638 13.4090 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_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.
;
_space_group_crystal_system monoclinic
_space_group_IT_number 14
_space_group_name_H-M_alt 'P 1 21/n 1'
_space_group_name_Hall '-P 2yn'
loop_
_space_group_symop_operation_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 13.8022(3)
_cell_length_b 16.3751(5)
_cell_length_c 18.0985(6)
_cell_angle_alpha 90
_cell_angle_beta 92.474(3)
_cell_angle_gamma 90
_cell_volume 4086.7(2)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 8669
_cell_measurement_temperature 120(2)
_cell_measurement_theta_max 74.8710
_cell_measurement_theta_min 3.7240
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 14.963
_exptl_absorpt_correction_T_max 0.263
_exptl_absorpt_correction_T_min 0.079
_exptl_absorpt_correction_type gaussian
_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)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour red
_exptl_crystal_colour_primary red
_exptl_crystal_density_diffrn 1.486
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 1844
_exptl_crystal_size_max 0.312
_exptl_crystal_size_mid 0.2502
_exptl_crystal_size_min 0.2097
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0615
_diffrn_reflns_av_unetI/netI 0.0612
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -17
_diffrn_reflns_limit_k_max 20
_diffrn_reflns_limit_k_min -16
_diffrn_reflns_limit_l_max 15
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 16902
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full 67.684
_diffrn_reflns_theta_max 75.005
_diffrn_reflns_theta_min 3.642
_diffrn_ambient_temperature 120(2)
_diffrn_detector_area_resol_mean 10.3613
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
1 omega -85.00 -8.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 125.0000 -30.0000 77
#__ type_ start__ end____ width___ exp.time_
2 omega -46.00 3.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 38.0000 -120.0000 49
#__ type_ start__ end____ width___ exp.time_
3 omega -98.00 -17.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- -38.5000 -77.0000 120.0000 81
#__ type_ start__ end____ width___ exp.time_
4 omega 61.00 89.00 1.0000 5.0000
omega____ theta____ kappa____ phi______ frames
- 43.1627 -125.0000 -180.0000 28
#__ type_ start__ end____ width___ exp.time_
5 omega 90.00 173.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 30.0000 -30.0000 83
#__ type_ start__ end____ width___ exp.time_
6 omega 118.00 153.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 125.0000 90.0000 35
#__ type_ start__ end____ width___ exp.time_
7 omega 42.00 91.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -30.0000 0.0000 49
#__ type_ start__ end____ width___ exp.time_
8 omega 38.00 120.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -125.0000 30.0000 82
#__ type_ start__ end____ width___ exp.time_
9 omega 55.00 89.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -45.0000 -30.0000 34
#__ type_ start__ end____ width___ exp.time_
10 omega 39.00 71.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -45.0000 60.0000 32
#__ type_ start__ end____ width___ exp.time_
11 omega 56.00 129.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -61.0000 -180.0000 73
#__ type_ start__ end____ width___ exp.time_
12 omega 28.00 102.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -95.0000 -150.0000 74
#__ type_ start__ end____ width___ exp.time_
13 omega 38.00 84.00 1.0000 25.0000
omega____ theta____ kappa____ phi______ frames
- 107.0972 -30.0000 60.0000 46
;
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_orient_matrix_UB_11 -0.0779384000
_diffrn_orient_matrix_UB_12 0.0107500000
_diffrn_orient_matrix_UB_13 0.0577042000
_diffrn_orient_matrix_UB_21 0.0191801000
_diffrn_orient_matrix_UB_22 0.0926270000
_diffrn_orient_matrix_UB_23 0.0015960000
_diffrn_orient_matrix_UB_31 -0.0777229000
_diffrn_orient_matrix_UB_32 0.0120243000
_diffrn_orient_matrix_UB_33 -0.0627287000
_diffrn_radiation_monochromator mirror
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54184
_diffrn_source 'SuperNova (Cu) X-ray Source'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 7122
_reflns_number_total 8115
_reflns_odcompleteness_completeness 99.66
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta 67.13
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_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 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'SHELXS-2012 (Sheldrick, 2012)'
_refine_diff_density_max 5.899
_refine_diff_density_min -2.262
_refine_diff_density_rms 0.337
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.143
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 680
_refine_ls_number_reflns 8115
_refine_ls_number_restraints 1911
_refine_ls_R_factor_all 0.0897
_refine_ls_R_factor_gt 0.0814
_refine_ls_restrained_S_all 1.056
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1138P)^2^+64.7301P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.2110
_refine_ls_wR_factor_ref 0.2190
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All C(H,H) groups
At 1.5 times of:
All C(H,H,H) groups
2. Restrained distances
Si2-N2 \\sim Si2A-N2 \\sim Si1-N1 \\sim Si1A-N1 \\sim Si3A-N3 \\sim Si3-N3
with sigma of 0.01
Si3A-C29A \\sim Si3-C29 \\sim Si3-C23 \\sim Si3A-C23A \\sim Si3-C26 \\sim
Si3A-C26A \\sim Si1-C4 ~
Si1A-C4A \\sim Si1-C1 \\sim Si1A-C1A \\sim Si1A-C7A \\sim Si1-C7 \\sim Si2-C18
\\sim Si2-C12 \\sim Si2A-
C12A \\sim Si2A-C18A \\sim Si2A-C15A \\sim Si2-C15
with sigma of 0.02
C19A-C18A \\sim C20A-C18A \\sim C19-C18 \\sim C20-C18 \\sim C13-C12 \\sim
C14-C12 \\sim C13A-C12A ~
C14A-C12A \\sim C16-C15 \\sim C17-C15 \\sim C17A-C15A \\sim C16A-C15A \\sim
C31-C29 \\sim C30-C29 ~
C30A-C29A \\sim C31A-C29A \\sim C28-C26 \\sim C27-C26 \\sim C28A-C26A \\sim
C27A-C26A \\sim C24A-C23A
\\sim C25A-C23A \\sim C25-C23 \\sim C24-C23 \\sim C8A-C7A \\sim C8-C7 \\sim
C9-C7 \\sim C9A-C7A \\sim C5A-C4A
\\sim C5-C4 \\sim C6A-C4A \\sim C6-C4 \\sim C2-C1 \\sim C2A-C1A \\sim C3-C1
\\sim C3A-C1A
with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Si1 \\sim Si1A \\sim C1 \\sim C2 \\sim C2A \\sim C4 \\sim C4A \\sim C5 \\sim
C5A \\sim C6 \\sim C6A \\sim C7 \\sim C7A \\sim C8 \\sim C8A \\sim C9 \\sim C9A
\\sim C1A \\sim C3 \\sim C3A \\sim Si2 \\sim C12 \\sim C12A \\sim C13 \\sim
C13A \\sim C14 \\sim C14A \\sim C15 \\sim C15A \\sim C16 \\sim C16A \\sim C17
\\sim C17A \\sim C18 \\sim C19 \\sim C18A \\sim C19A \\sim C20 \\sim C20A \\sim
Si2A \\sim Si3 \\sim Si3A \\sim C23 \\sim C23A \\sim C24 \\sim C24A \\sim C25
\\sim C25A \\sim C26 \\sim C26A \\sim C27 \\sim C27A \\sim C28 \\sim C28A \\sim
C29 \\sim C29A \\sim C30 \\sim C30A \\sim C31 \\sim C31A: within 2A with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
Si2, Si2A, C12, C12A, C13, C13A, C14, C14A, C15, C15A, C16, C16A, C17, C17A,
C18, C18A, C19, C19A, C20, C20A, Si3, C25, C26, C26A, C28, C28A, C29, C29A,
C30, C30A, C31, C31A, Si3A, C23, C23A, C24, C24A, C25A, C27, C27A, Si1, Si1A,
C1, C1A, C2, C2A, C3, C3A, C4, C4A, C5, C5A, C6, C6A, C7, C7A, C8, C8A, C9,
C9A, N2
with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
Sof(Si3A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24D)=Sof(H24E)=Sof(H24F)=
Sof(C25A)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(C26A)=Sof(H26A)=Sof(C27A)=
Sof(H27D)=Sof(H27E)=Sof(H27F)=Sof(C28A)=Sof(H28D)=Sof(H28E)=Sof(H28F)=
Sof(C29A)=Sof(H29A)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(C31A)=
Sof(H31D)=Sof(H31E)=Sof(H31F)=1-FVAR(1)
Sof(Si3)=Sof(C23)=Sof(H23)=Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C25)=
Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C26)=Sof(H26)=Sof(C27)=Sof(H27A)=Sof(H27B)=
Sof(H27C)=Sof(C28)=Sof(H28A)=Sof(H28B)=Sof(H28C)=Sof(C29)=Sof(H29)=Sof(C30)=
Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C31)=Sof(H31A)=Sof(H31B)=Sof(H31C)=FVAR(1)
Sof(Si1A)=Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2AA)=Sof(H2AB)=Sof(H2AC)=Sof(C3A)=
Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AA)=Sof(H5AB)=
Sof(H5AC)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(H6AC)=Sof(C7A)=Sof(H7A)=Sof(C8A)=
Sof(H8AA)=Sof(H8AB)=Sof(H8AC)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
Sof(Si1)=Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=Sof(C3)=Sof(H3A)=
Sof(H3B)=Sof(H3C)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5A)=Sof(H5B)=Sof(H5C)=Sof(C6)=
Sof(H6A)=Sof(H6B)=Sof(H6C)=Sof(C7)=Sof(H7)=Sof(C8)=Sof(H8A)=Sof(H8B)=Sof(H8C)=
Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
Sof(Si2A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(H13D)=Sof(H13E)=Sof(H13F)=
Sof(C14A)=Sof(H14D)=Sof(H14E)=Sof(H14F)=Sof(C15A)=Sof(H15A)=Sof(C16A)=
Sof(H16D)=Sof(H16E)=Sof(H16F)=Sof(C17A)=Sof(H17D)=Sof(H17E)=Sof(H17F)=
Sof(C18A)=Sof(H18A)=Sof(C19A)=Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(C20A)=
Sof(H20D)=Sof(H20E)=Sof(H20F)=1-FVAR(3)
Sof(Si2)=Sof(C12)=Sof(H12)=Sof(C13)=Sof(H13A)=Sof(H13B)=Sof(H13C)=Sof(C14)=
Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16A)=Sof(H16B)=
Sof(H16C)=Sof(C17)=Sof(H17A)=Sof(H17B)=Sof(H17C)=Sof(C18)=Sof(H18)=Sof(C19)=
Sof(H19A)=Sof(H19B)=Sof(H19C)=Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(H20C)=FVAR(3)
6.a Ternary CH refined with riding coordinates:
C1(H1), C1A(H1A), C4(H4), C4A(H4A), C7(H7), C7A(H7A), C12(H12), C12A(H12A),
C15(H15), C15A(H15A), C18(H18), C18A(H18A), C23(H23), C23A(H23A), C26(H26),
C26A(H26A), C29(H29), C29A(H29A)
6.b Secondary CH2 refined with riding coordinates:
C10(H10A,H10B), C11(H11A,H11B), C21(H21A,H21B), C22(H22A,H22B), C32(H32A,
H32B), C33(H33A,H33B)
6.c Idealised Me refined as rotating group:
C2(H2A,H2B,H2C), C2A(H2AA,H2AB,H2AC), C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC),
C5(H5A,H5B,H5C), C5A(H5AA,H5AB,H5AC), C6(H6A,H6B,H6C), C6A(H6AA,H6AB,H6AC),
C8(H8A,H8B,H8C), C8A(H8AA,H8AB,H8AC), C9(H9A,H9B,H9C), C9A(H9AA,H9AB,H9AC),
C13(H13A,H13B,H13C), C13A(H13D,H13E,H13F), C14(H14A,H14B,H14C), C14A(H14D,H14E,
H14F), C16(H16A,H16B,H16C), C16A(H16D,H16E,H16F), C17(H17A,H17B,H17C),
C17A(H17D,H17E,H17F), C19(H19A,H19B,H19C), C19A(H19D,H19E,H19F), C20(H20A,H20B,
H20C), C20A(H20D,H20E,H20F), C24(H24A,H24B,H24C), C24A(H24D,H24E,H24F),
C25(H25A,H25B,H25C), C25A(H25D,H25E,H25F), C27(H27A,H27B,H27C), C27A(H27D,H27E,
H27F), C28(H28A,H28B,H28C), C28A(H28D,H28E,H28F), C30(H30A,H30B,H30C),
C30A(H30D,H30E,H30F), C31(H31A,H31B,H31C), C31A(H31D,H31E,H31F)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
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
U1 U 0.06059(3) 0.85197(2) 0.09636(2) 0.02857(17) Uani 1 1 d . . . . .
Te1 Te 0.000000 1.000000 0.000000 0.0374(3) Uani 1 2 d S T P . .
N1 N 0.0215(8) 0.7350(6) 0.0402(6) 0.040(2) Uani 1 1 d D . . . .
Si1 Si -0.0595(8) 0.6910(7) -0.0268(5) 0.033(2) Uani 0.448(15) 1 d D U . A 1
Si1A Si -0.0861(6) 0.7041(6) -0.0122(5) 0.0353(18) Uani 0.552(15) 1 d D U . A 2
C1 C -0.1504(18) 0.7775(14) -0.0377(13) 0.035(3) Uani 0.448(15) 1 d D U . A 1
H1 H -0.114525 0.825576 -0.053563 0.042 Uiso 0.448(15) 1 calc R . . A 1
C1A C -0.1845(14) 0.7855(12) -0.0176(11) 0.035(3) Uani 0.552(15) 1 d D U . A 2
H1A H -0.159381 0.829515 -0.048143 0.042 Uiso 0.552(15) 1 calc R . . A 2
C2 C -0.230(2) 0.762(2) -0.0966(16) 0.048(5) Uani 0.448(15) 1 d D U . A 1
H2A H -0.201091 0.741746 -0.140592 0.072 Uiso 0.448(15) 1 calc GR . . A 1
H2B H -0.263893 0.811475 -0.107546 0.072 Uiso 0.448(15) 1 calc GR . . A 1
H2C H -0.273878 0.721612 -0.078992 0.072 Uiso 0.448(15) 1 calc GR . . A 1
C2A C -0.2766(18) 0.7551(16) -0.0585(13) 0.044(4) Uani 0.552(15) 1 d D U . A 2
H2AA H -0.260010 0.730124 -0.104257 0.067 Uiso 0.552(15) 1 calc GR . . A 2
H2AB H -0.319417 0.800338 -0.068551 0.067 Uiso 0.552(15) 1 calc GR . . A 2
H2AC H -0.308162 0.715795 -0.028455 0.067 Uiso 0.552(15) 1 calc GR . . A 2
C3 C -0.200(2) 0.802(2) 0.0322(15) 0.038(5) Uani 0.448(15) 1 d D U . A 1
H3A H -0.234970 0.755533 0.050570 0.056 Uiso 0.448(15) 1 calc GR . . A 1
H3B H -0.245229 0.845330 0.021236 0.056 Uiso 0.448(15) 1 calc GR . . A 1
H3C H -0.152832 0.819411 0.068967 0.056 Uiso 0.448(15) 1 calc GR . . A 1
C3A C -0.2063(18) 0.8245(17) 0.0561(12) 0.036(4) Uani 0.552(15) 1 d D U . A 2
H3AA H -0.212209 0.782654 0.092747 0.054 Uiso 0.552(15) 1 calc GR . . A 2
H3AB H -0.265934 0.854559 0.051045 0.054 Uiso 0.552(15) 1 calc GR . . A 2
H3AC H -0.154508 0.860867 0.070931 0.054 Uiso 0.552(15) 1 calc GR . . A 2
C4 C -0.108(2) 0.5887(13) 0.0065(12) 0.034(3) Uani 0.448(15) 1 d D U . A 1
H4 H -0.051183 0.553526 0.015861 0.041 Uiso 0.448(15) 1 calc R . . A 1
C4A C -0.1351(18) 0.6043(11) 0.0267(10) 0.036(3) Uani 0.552(15) 1 d D U . A 2
H4A H -0.077524 0.572713 0.042331 0.043 Uiso 0.552(15) 1 calc R . . A 2
C5 C -0.161(3) 0.592(2) 0.0782(15) 0.040(5) Uani 0.448(15) 1 d D U . A 1
H5A H -0.127301 0.627613 0.112583 0.060 Uiso 0.448(15) 1 calc GR . . A 1
H5B H -0.164216 0.538106 0.098984 0.060 Uiso 0.448(15) 1 calc GR . . A 1
H5C H -0.225761 0.612136 0.068364 0.060 Uiso 0.448(15) 1 calc GR . . A 1
C5A C -0.193(2) 0.6132(18) 0.0959(13) 0.043(5) Uani 0.552(15) 1 d D U . A 2
H5AA H -0.252941 0.641046 0.083723 0.064 Uiso 0.552(15) 1 calc GR . . A 2
H5AB H -0.156274 0.644015 0.132417 0.064 Uiso 0.552(15) 1 calc GR . . A 2
H5AC H -0.206944 0.560037 0.115279 0.064 Uiso 0.552(15) 1 calc GR . . A 2
C6 C -0.171(2) 0.547(2) -0.0528(16) 0.037(5) Uani 0.448(15) 1 d D U . A 1
H6A H -0.228441 0.578419 -0.063000 0.055 Uiso 0.448(15) 1 calc GR . . A 1
H6B H -0.188899 0.493375 -0.035726 0.055 Uiso 0.448(15) 1 calc GR . . A 1
H6C H -0.135680 0.541269 -0.097068 0.055 Uiso 0.448(15) 1 calc GR . . A 1
C6A C -0.192(2) 0.5494(17) -0.0279(13) 0.039(5) Uani 0.552(15) 1 d D U . A 2
H6AA H -0.258941 0.564976 -0.029828 0.058 Uiso 0.552(15) 1 calc GR . . A 2
H6AB H -0.185942 0.493569 -0.012085 0.058 Uiso 0.552(15) 1 calc GR . . A 2
H6AC H -0.166269 0.555027 -0.076137 0.058 Uiso 0.552(15) 1 calc GR . . A 2
C7 C -0.004(2) 0.6691(14) -0.1187(11) 0.038(3) Uani 0.448(15) 1 d D U . A 1
H7 H -0.059055 0.655975 -0.152640 0.045 Uiso 0.448(15) 1 calc R . . A 1
C7A C -0.052(2) 0.6811(12) -0.1108(9) 0.040(3) Uani 0.552(15) 1 d D U . A 2
H7A H -0.109058 0.653386 -0.133555 0.048 Uiso 0.552(15) 1 calc R . . A 2
C8 C 0.041(3) 0.7451(17) -0.1508(16) 0.049(5) Uani 0.448(15) 1 d D U . A 1
H8A H -0.006371 0.787892 -0.154517 0.073 Uiso 0.448(15) 1 calc GR . . A 1
H8B H 0.063643 0.733055 -0.199069 0.073 Uiso 0.448(15) 1 calc GR . . A 1
H8C H 0.094852 0.762508 -0.119128 0.073 Uiso 0.448(15) 1 calc GR . . A 1
C8A C -0.041(2) 0.7582(14) -0.1557(13) 0.048(4) Uani 0.552(15) 1 d D U . A 2
H8AA H -0.100439 0.788525 -0.156866 0.071 Uiso 0.552(15) 1 calc GR . . A 2
H8AB H -0.025020 0.744144 -0.205260 0.071 Uiso 0.552(15) 1 calc GR . . A 2
H8AC H 0.010223 0.791002 -0.133499 0.071 Uiso 0.552(15) 1 calc GR . . A 2
C9 C 0.064(3) 0.597(2) -0.124(2) 0.047(5) Uani 0.448(15) 1 d D U . A 1
H9A H 0.123334 0.608980 -0.095719 0.071 Uiso 0.448(15) 1 calc GR . . A 1
H9B H 0.078316 0.588107 -0.174466 0.071 Uiso 0.448(15) 1 calc GR . . A 1
H9C H 0.034419 0.549616 -0.103998 0.071 Uiso 0.448(15) 1 calc GR . . A 1
C9A C 0.031(2) 0.6202(18) -0.1159(15) 0.048(4) Uani 0.552(15) 1 d D U . A 2
H9AA H 0.088900 0.643637 -0.094247 0.071 Uiso 0.552(15) 1 calc GR . . A 2
H9AB H 0.039947 0.607433 -0.166843 0.071 Uiso 0.552(15) 1 calc GR . . A 2
H9AC H 0.015058 0.571251 -0.089742 0.071 Uiso 0.552(15) 1 calc GR . . A 2
C10 C 0.0935(13) 0.6689(10) 0.0593(8) 0.051(4) Uani 1 1 d . . . . .
H10A H 0.158574 0.687432 0.049779 0.061 Uiso 1 1 calc R . . . .
H10B H 0.079695 0.620910 0.029193 0.061 Uiso 1 1 calc R . . . .
C11 C 0.0861(15) 0.6480(8) 0.1412(8) 0.051(4) Uani 1 1 d . . . . .
H11A H 0.021334 0.628635 0.150577 0.061 Uiso 1 1 calc R . . . .
H11B H 0.132045 0.605334 0.155197 0.061 Uiso 1 1 calc R . . . .
N2 N -0.0168(8) 0.8612(7) 0.2001(6) 0.049(3) Uani 1 1 d D U . . .
Si2 Si -0.0493(5) 0.9536(5) 0.2492(4) 0.0375(15) Uani 0.515(10) 1 d D U . B 1
Si2A Si -0.0804(5) 0.9216(5) 0.2600(4) 0.0343(15) Uani 0.485(10) 1 d D U . B 2
C12 C 0.0288(16) 1.0456(12) 0.2283(13) 0.042(3) Uani 0.515(10) 1 d D U . B 1
H12 H -0.000725 1.070573 0.183616 0.051 Uiso 0.515(10) 1 calc R . . B 1
C12A C -0.0296(16) 1.0251(11) 0.2350(13) 0.041(3) Uani 0.485(10) 1 d D U . B 2
H12A H -0.052284 1.036429 0.183968 0.049 Uiso 0.485(10) 1 calc R . . B 2
C13 C 0.033(2) 1.1124(17) 0.2869(15) 0.051(4) Uani 0.515(10) 1 d D U . B 1
H13A H -0.032141 1.126563 0.299429 0.077 Uiso 0.515(10) 1 calc GR . . B 1
H13B H 0.064310 1.159719 0.267924 0.077 Uiso 0.515(10) 1 calc GR . . B 1
H13C H 0.068097 1.093158 0.330239 0.077 Uiso 0.515(10) 1 calc GR . . B 1
C13A C -0.068(2) 1.0934(18) 0.2825(16) 0.052(5) Uani 0.485(10) 1 d D U . B 2
H13D H -0.043371 1.086839 0.332537 0.078 Uiso 0.485(10) 1 calc GR . . B 2
H13E H -0.137523 1.091506 0.281072 0.078 Uiso 0.485(10) 1 calc GR . . B 2
H13F H -0.047180 1.145120 0.263754 0.078 Uiso 0.485(10) 1 calc GR . . B 2
C14 C 0.1336(16) 1.0264(16) 0.2105(16) 0.042(4) Uani 0.515(10) 1 d D U . B 1
H14A H 0.169208 1.010401 0.254875 0.063 Uiso 0.515(10) 1 calc GR . . B 1
H14B H 0.163020 1.073996 0.190097 0.063 Uiso 0.515(10) 1 calc GR . . B 1
H14C H 0.134482 0.982623 0.175175 0.063 Uiso 0.515(10) 1 calc GR . . B 1
C14A C 0.0803(17) 1.0272(18) 0.2363(18) 0.043(4) Uani 0.485(10) 1 d D U . B 2
H14D H 0.105613 1.014997 0.285247 0.064 Uiso 0.485(10) 1 calc GR . . B 2
H14E H 0.101519 1.080522 0.222038 0.064 Uiso 0.485(10) 1 calc GR . . B 2
H14F H 0.103282 0.987342 0.202263 0.064 Uiso 0.485(10) 1 calc GR . . B 2
C15 C -0.0403(15) 0.9311(17) 0.3528(8) 0.039(3) Uani 0.515(10) 1 d D U . B 1
H15 H -0.067862 0.876366 0.357645 0.046 Uiso 0.515(10) 1 calc R . . B 1
C15A C -0.0571(15) 0.8912(17) 0.3604(8) 0.036(3) Uani 0.485(10) 1 d D U . B 2
H15A H -0.068738 0.832285 0.362986 0.043 Uiso 0.485(10) 1 calc R . . B 2
C16 C -0.0977(19) 0.9845(16) 0.4042(12) 0.040(4) Uani 0.515(10) 1 d D U . B 1
H16A H -0.071888 1.038957 0.404462 0.060 Uiso 0.515(10) 1 calc GR . . B 1
H16B H -0.092883 0.962469 0.453345 0.060 Uiso 0.515(10) 1 calc GR . . B 1
H16C H -0.164503 0.985737 0.387097 0.060 Uiso 0.515(10) 1 calc GR . . B 1
C16A C -0.1283(18) 0.9308(17) 0.4109(14) 0.039(4) Uiso 0.485(10) 1 d D U . B 2
H16D H -0.129022 0.988768 0.402692 0.059 Uiso 0.485(10) 1 calc GR . . B 2
H16E H -0.108911 0.919823 0.461465 0.059 Uiso 0.485(10) 1 calc GR . . B 2
H16F H -0.191935 0.909028 0.400369 0.059 Uiso 0.485(10) 1 calc GR . . B 2
C17 C 0.0647(17) 0.923(2) 0.3820(19) 0.037(5) Uani 0.515(10) 1 d D U . B 1
H17A H 0.099396 0.887734 0.350047 0.056 Uiso 0.515(10) 1 calc GR . . B 1
H17B H 0.066030 0.900259 0.430973 0.056 Uiso 0.515(10) 1 calc GR . . B 1
H17C H 0.094799 0.975873 0.383527 0.056 Uiso 0.515(10) 1 calc GR . . B 1
C17A C 0.0455(18) 0.905(3) 0.392(2) 0.040(5) Uani 0.485(10) 1 d D U . B 2
H17D H 0.091107 0.884077 0.358181 0.060 Uiso 0.485(10) 1 calc GR . . B 2
H17E H 0.053834 0.877540 0.438571 0.060 Uiso 0.485(10) 1 calc GR . . B 2
H17F H 0.056330 0.962587 0.398928 0.060 Uiso 0.485(10) 1 calc GR . . B 2
C18 C -0.1794(11) 0.9842(13) 0.2208(13) 0.039(3) Uani 0.515(10) 1 d D U . B 1
H18 H -0.181639 0.984325 0.166584 0.047 Uiso 0.515(10) 1 calc R . . B 1
C18A C -0.2157(11) 0.9242(15) 0.2388(14) 0.039(3) Uani 0.485(10) 1 d D U . B 2
H18A H -0.244290 0.954472 0.279238 0.046 Uiso 0.485(10) 1 calc R . . B 2
C19 C -0.2132(19) 1.0691(14) 0.2423(13) 0.043(4) Uani 0.515(10) 1 d D U . B 1
H19A H -0.215595 1.072583 0.295177 0.065 Uiso 0.515(10) 1 calc GR . . B 1
H19B H -0.276569 1.079136 0.220303 0.065 Uiso 0.515(10) 1 calc GR . . B 1
H19C H -0.168646 1.109202 0.225130 0.065 Uiso 0.515(10) 1 calc GR . . B 1
C19A C -0.241(2) 0.972(2) 0.1682(13) 0.044(4) Uani 0.485(10) 1 d D U . B 2
H19D H -0.209046 1.023611 0.170104 0.067 Uiso 0.485(10) 1 calc GR . . B 2
H19E H -0.309832 0.979469 0.163433 0.067 Uiso 0.485(10) 1 calc GR . . B 2
H19F H -0.219809 0.941247 0.126365 0.067 Uiso 0.485(10) 1 calc GR . . B 2
C20 C -0.254(2) 0.9204(19) 0.2418(17) 0.048(4) Uani 0.515(10) 1 d D U . B 1
H20A H -0.317727 0.940849 0.230899 0.072 Uiso 0.515(10) 1 calc GR . . B 1
H20B H -0.245790 0.908775 0.293739 0.072 Uiso 0.515(10) 1 calc GR . . B 1
H20C H -0.243779 0.871306 0.214111 0.072 Uiso 0.515(10) 1 calc GR . . B 1
C20A C -0.262(2) 0.8401(17) 0.2375(17) 0.047(5) Uani 0.485(10) 1 d D U . B 2
H20D H -0.238069 0.808793 0.197490 0.071 Uiso 0.485(10) 1 calc GR . . B 2
H20E H -0.331480 0.845668 0.230809 0.071 Uiso 0.485(10) 1 calc GR . . B 2
H20F H -0.247187 0.812680 0.283458 0.071 Uiso 0.485(10) 1 calc GR . . B 2
C21 C -0.0437(10) 0.7750(14) 0.2258(7) 0.061(5) Uani 1 1 d . . . . .
H21A H -0.086979 0.778561 0.266491 0.074 Uiso 1 1 calc R . . . .
H21B H -0.076998 0.745755 0.185547 0.074 Uiso 1 1 calc R . . . .
C22 C 0.0452(11) 0.7307(11) 0.2497(7) 0.052(4) Uani 1 1 d . . . . .
H22A H 0.028813 0.676778 0.267609 0.063 Uiso 1 1 calc R . . . .
H22B H 0.079155 0.760076 0.289448 0.063 Uiso 1 1 calc R . . . .
N3 N 0.2180(7) 0.8503(7) 0.1249(7) 0.049(3) Uani 1 1 d D . . . .
Si3 Si 0.3255(5) 0.8907(5) 0.0905(4) 0.0341(15) Uani 0.499(10) 1 d D U . C 1
Si3A Si 0.3237(5) 0.8564(6) 0.0697(5) 0.0420(17) Uani 0.501(10) 1 d D U . C 2
C23 C 0.2821(16) 0.9254(14) -0.0054(9) 0.040(3) Uani 0.499(10) 1 d D U . C 1
H23 H 0.235643 0.969819 0.001247 0.048 Uiso 0.499(10) 1 calc R . . C 1
C23A C 0.2931(16) 0.8683(16) -0.0337(9) 0.044(3) Uani 0.501(10) 1 d D U . C 2
H23A H 0.261458 0.921633 -0.039512 0.052 Uiso 0.501(10) 1 calc R . . C 2
C24 C 0.229(2) 0.8591(16) -0.0504(15) 0.044(5) Uani 0.499(10) 1 d D U . C 1
H24A H 0.274809 0.818110 -0.064198 0.067 Uiso 0.499(10) 1 calc GR . . C 1
H24B H 0.199091 0.882759 -0.094136 0.067 Uiso 0.499(10) 1 calc GR . . C 1
H24C H 0.180567 0.834622 -0.021215 0.067 Uiso 0.499(10) 1 calc GR . . C 1
C24A C 0.2224(19) 0.8065(17) -0.0678(16) 0.045(5) Uani 0.501(10) 1 d D U . C 2
H24D H 0.254253 0.754627 -0.071878 0.068 Uiso 0.501(10) 1 calc GR . . C 2
H24E H 0.200533 0.824784 -0.116055 0.068 Uiso 0.501(10) 1 calc GR . . C 2
H24F H 0.167896 0.800895 -0.037021 0.068 Uiso 0.501(10) 1 calc GR . . C 2
C25 C 0.3633(19) 0.960(2) -0.0504(17) 0.052(5) Uani 0.499(10) 1 d D U . C 1
H25A H 0.387800 1.008928 -0.027680 0.078 Uiso 0.499(10) 1 calc GR . . C 1
H25B H 0.338717 0.971526 -0.099717 0.078 Uiso 0.499(10) 1 calc GR . . C 1
H25C H 0.414626 0.920300 -0.052388 0.078 Uiso 0.499(10) 1 calc GR . . C 1
C25A C 0.381(2) 0.871(2) -0.0822(19) 0.056(5) Uani 0.501(10) 1 d D U . C 2
H25D H 0.423735 0.913780 -0.065693 0.084 Uiso 0.501(10) 1 calc GR . . C 2
H25E H 0.359549 0.880503 -0.132651 0.084 Uiso 0.501(10) 1 calc GR . . C 2
H25F H 0.414423 0.819432 -0.078866 0.084 Uiso 0.501(10) 1 calc GR . . C 2
C26 C 0.4215(13) 0.8074(12) 0.0929(17) 0.044(3) Uani 0.499(10) 1 d D U . C 1
H26 H 0.425909 0.787085 0.143888 0.053 Uiso 0.499(10) 1 calc R . . C 1
C26A C 0.4114(14) 0.7678(12) 0.0876(18) 0.048(3) Uani 0.501(10) 1 d D U . C 2
H26A H 0.405939 0.752969 0.139678 0.057 Uiso 0.501(10) 1 calc R . . C 2
C27 C 0.398(2) 0.7342(18) 0.0443(19) 0.051(5) Uani 0.499(10) 1 d D U . C 1
H27A H 0.343926 0.705361 0.063059 0.076 Uiso 0.499(10) 1 calc GR . . C 1
H27B H 0.453408 0.698649 0.044125 0.076 Uiso 0.499(10) 1 calc GR . . C 1
H27C H 0.382336 0.752313 -0.005259 0.076 Uiso 0.499(10) 1 calc GR . . C 1
C27A C 0.387(2) 0.6906(17) 0.043(2) 0.054(5) Uani 0.501(10) 1 d D U . C 2
H27D H 0.319825 0.676619 0.048915 0.081 Uiso 0.501(10) 1 calc GR . . C 2
H27E H 0.427153 0.646447 0.060857 0.081 Uiso 0.501(10) 1 calc GR . . C 2
H27F H 0.397404 0.700123 -0.008170 0.081 Uiso 0.501(10) 1 calc GR . . C 2
C28 C 0.5225(17) 0.837(2) 0.076(2) 0.052(5) Uani 0.499(10) 1 d D U . C 1
H28A H 0.517601 0.888122 0.049628 0.078 Uiso 0.499(10) 1 calc GR . . C 1
H28B H 0.553328 0.797424 0.045536 0.078 Uiso 0.499(10) 1 calc GR . . C 1
H28C H 0.560217 0.844537 0.120984 0.078 Uiso 0.499(10) 1 calc GR . . C 1
C28A C 0.5181(16) 0.786(2) 0.078(2) 0.054(5) Uani 0.501(10) 1 d D U . C 2
H28D H 0.525997 0.808912 0.029428 0.080 Uiso 0.501(10) 1 calc GR . . C 2
H28E H 0.554812 0.736401 0.082498 0.080 Uiso 0.501(10) 1 calc GR . . C 2
H28F H 0.540687 0.824279 0.114671 0.080 Uiso 0.501(10) 1 calc GR . . C 2
C29 C 0.3840(16) 0.9807(11) 0.1397(13) 0.040(3) Uani 0.499(10) 1 d D U . C 1
H29 H 0.435186 0.999793 0.108012 0.048 Uiso 0.499(10) 1 calc R . . C 1
C29A C 0.3972(16) 0.9519(10) 0.0936(14) 0.042(3) Uani 0.501(10) 1 d D U . C 2
H29A H 0.458660 0.948656 0.068553 0.050 Uiso 0.501(10) 1 calc R . . C 2
C30 C 0.433(2) 0.9655(19) 0.2153(15) 0.048(5) Uani 0.499(10) 1 d D U . C 1
H30A H 0.386765 0.973841 0.252834 0.073 Uiso 0.499(10) 1 calc GR . . C 1
H30B H 0.486036 1.002737 0.222955 0.073 Uiso 0.499(10) 1 calc GR . . C 1
H30C H 0.456416 0.910424 0.217783 0.073 Uiso 0.499(10) 1 calc GR . . C 1
C30A C 0.420(2) 0.958(2) 0.1761(14) 0.049(5) Uani 0.501(10) 1 d D U . C 2
H30D H 0.361375 0.970015 0.200921 0.074 Uiso 0.501(10) 1 calc GR . . C 2
H30E H 0.465953 1.001297 0.185572 0.074 Uiso 0.501(10) 1 calc GR . . C 2
H30F H 0.446539 0.907506 0.194035 0.074 Uiso 0.501(10) 1 calc GR . . C 2
C31 C 0.3117(18) 1.0505(15) 0.143(2) 0.051(5) Uani 0.499(10) 1 d D U . C 1
H31A H 0.256331 1.038968 0.111056 0.076 Uiso 0.499(10) 1 calc GR . . C 1
H31B H 0.341677 1.100249 0.128021 0.076 Uiso 0.499(10) 1 calc GR . . C 1
H31C H 0.291390 1.056301 0.193102 0.076 Uiso 0.499(10) 1 calc GR . . C 1
C31A C 0.3451(19) 1.0291(14) 0.0682(18) 0.045(4) Uani 0.501(10) 1 d D U . C 2
H31D H 0.354458 1.037584 0.016554 0.068 Uiso 0.501(10) 1 calc GR . . C 2
H31E H 0.370717 1.074849 0.095908 0.068 Uiso 0.501(10) 1 calc GR . . C 2
H31F H 0.277058 1.023784 0.076209 0.068 Uiso 0.501(10) 1 calc GR . . C 2
C32 C 0.2378(11) 0.8218(10) 0.2032(9) 0.049(3) Uani 1 1 d . . . . .
H32A H 0.198482 0.852431 0.236710 0.059 Uiso 1 1 calc R . . . .
H32B H 0.305531 0.830202 0.217702 0.059 Uiso 1 1 calc R . . . .
C33 C 0.2125(10) 0.7304(9) 0.2065(9) 0.046(3) Uani 1 1 d . . . . .
H33A H 0.250958 0.699699 0.172503 0.056 Uiso 1 1 calc R . . . .
H33B H 0.225178 0.709352 0.256023 0.056 Uiso 1 1 calc R . . . .
N4 N 0.1078(8) 0.7235(7) 0.1851(6) 0.042(2) Uani 1 1 d . . . . .
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
U1 0.0267(2) 0.0311(2) 0.0272(2) 0.00171(13) -0.00697(15) -0.00130(13)
Te1 0.0389(6) 0.0284(5) 0.0433(6) 0.0050(4) -0.0149(4) 0.0024(4)
N1 0.064(7) 0.014(4) 0.042(6) 0.000(4) -0.005(5) -0.008(4)
Si1 0.057(4) 0.023(4) 0.018(4) -0.005(3) 0.005(3) -0.006(3)
Si1A 0.060(4) 0.029(3) 0.016(3) -0.004(2) -0.006(3) -0.006(3)
C1 0.055(6) 0.031(5) 0.019(6) -0.002(5) -0.004(5) -0.004(5)
C1A 0.052(6) 0.035(6) 0.019(6) 0.001(5) -0.009(5) -0.003(5)
C2 0.065(10) 0.050(10) 0.028(9) -0.005(9) -0.014(8) 0.004(9)
C2A 0.060(9) 0.042(9) 0.029(8) 0.004(7) -0.019(7) -0.004(8)
C3 0.043(9) 0.047(11) 0.021(8) -0.006(8) -0.010(8) 0.004(8)
C3A 0.033(9) 0.046(11) 0.028(9) -0.007(7) -0.011(7) -0.004(8)
C4 0.058(6) 0.027(5) 0.018(6) -0.004(5) 0.002(5) -0.009(5)
C4A 0.055(7) 0.031(6) 0.022(6) -0.003(5) 0.001(5) -0.007(5)
C5 0.060(11) 0.034(10) 0.026(8) -0.010(8) 0.006(7) -0.012(9)
C5A 0.056(11) 0.044(11) 0.028(8) -0.007(8) 0.006(7) -0.014(9)
C6 0.053(11) 0.037(9) 0.021(9) -0.007(9) 0.006(8) -0.017(8)
C6A 0.059(10) 0.037(8) 0.021(9) -0.006(8) 0.007(8) -0.011(8)
C7 0.058(7) 0.030(6) 0.027(5) -0.003(5) 0.009(6) 0.000(6)
C7A 0.061(6) 0.033(5) 0.027(5) -0.002(4) 0.005(5) -0.007(5)
C8 0.076(11) 0.040(8) 0.031(9) 0.000(8) 0.015(9) -0.008(9)
C8A 0.072(11) 0.038(8) 0.033(8) 0.001(7) 0.000(8) -0.009(8)
C9 0.057(13) 0.042(10) 0.044(11) 0.003(9) 0.014(10) 0.012(9)
C9A 0.067(11) 0.040(9) 0.036(9) -0.006(8) 0.006(8) -0.001(7)
C10 0.071(10) 0.046(8) 0.035(7) 0.003(6) -0.008(7) 0.000(7)
C11 0.088(12) 0.023(6) 0.040(7) 0.004(5) -0.017(7) -0.004(6)
N2 0.034(5) 0.089(7) 0.025(5) -0.001(5) -0.004(4) 0.018(5)
Si2 0.029(3) 0.057(4) 0.025(3) 0.009(3) -0.006(2) -0.002(3)
Si2A 0.027(3) 0.052(4) 0.024(3) 0.011(3) 0.003(2) -0.002(3)
C12 0.035(6) 0.054(6) 0.037(6) 0.009(5) -0.006(6) -0.003(5)
C12A 0.036(5) 0.054(5) 0.033(5) 0.011(5) -0.002(5) -0.005(5)
C13 0.051(9) 0.051(8) 0.051(9) 0.002(7) -0.007(8) -0.008(8)
C13A 0.055(10) 0.054(8) 0.046(9) 0.008(8) 0.001(9) 0.000(8)
C14 0.036(8) 0.033(9) 0.058(11) 0.021(8) -0.007(8) -0.002(7)
C14A 0.037(7) 0.037(9) 0.053(9) 0.010(8) -0.005(8) -0.010(7)
C15 0.035(5) 0.053(6) 0.027(4) 0.004(5) -0.004(4) 0.000(5)
C15A 0.034(6) 0.049(7) 0.025(5) 0.009(5) -0.001(5) -0.001(6)
C16 0.044(9) 0.047(9) 0.029(7) 0.004(7) -0.005(7) 0.004(7)
C17 0.038(8) 0.049(12) 0.024(9) 0.009(9) -0.008(8) -0.003(8)
C17A 0.039(9) 0.056(12) 0.024(9) 0.009(9) -0.004(8) -0.002(9)
C18 0.030(5) 0.056(6) 0.030(5) 0.007(5) -0.003(5) 0.004(5)
C18A 0.026(5) 0.059(6) 0.031(6) 0.004(6) 0.003(5) 0.003(5)
C19 0.040(10) 0.061(8) 0.028(10) 0.002(8) -0.004(8) 0.009(8)
C19A 0.035(9) 0.059(10) 0.039(8) 0.003(7) -0.001(7) 0.013(8)
C20 0.037(8) 0.065(8) 0.042(9) 0.004(8) 0.001(8) -0.001(8)
C20A 0.034(9) 0.065(9) 0.043(11) 0.005(9) -0.002(9) -0.004(8)
C21 0.036(7) 0.126(16) 0.023(6) 0.020(7) 0.002(5) -0.030(8)
C22 0.054(8) 0.073(10) 0.028(6) 0.005(6) -0.010(6) -0.024(8)
N3 0.031(6) 0.046(7) 0.069(8) 0.021(6) -0.017(5) -0.004(5)
Si3 0.030(3) 0.030(4) 0.041(3) 0.001(3) -0.009(2) -0.005(3)
Si3A 0.029(3) 0.030(4) 0.065(4) 0.014(3) -0.014(3) -0.008(3)
C23 0.033(5) 0.037(6) 0.049(5) 0.009(5) -0.006(5) -0.009(5)
C23A 0.034(6) 0.037(6) 0.059(6) 0.011(5) -0.005(5) -0.007(6)
C24 0.046(9) 0.046(9) 0.040(9) 0.001(8) -0.007(8) -0.008(8)
C24A 0.043(9) 0.042(10) 0.050(10) 0.004(9) 0.001(8) -0.006(8)
C25 0.043(9) 0.055(10) 0.058(9) 0.013(9) 0.002(8) -0.011(8)
C25A 0.044(9) 0.052(12) 0.073(11) 0.013(11) 0.007(9) -0.001(9)
C26 0.034(5) 0.033(6) 0.065(6) 0.000(6) -0.010(5) -0.002(5)
C26A 0.034(6) 0.035(6) 0.074(7) 0.009(6) -0.010(6) -0.002(5)
C27 0.041(9) 0.035(8) 0.076(10) -0.006(8) -0.004(9) 0.003(7)
C27A 0.044(10) 0.036(9) 0.082(12) 0.009(9) -0.009(10) -0.002(8)
C28 0.035(7) 0.040(10) 0.081(11) -0.006(10) -0.001(8) 0.001(7)
C28A 0.037(7) 0.038(9) 0.085(11) 0.006(9) -0.005(8) 0.003(7)
C29 0.037(6) 0.033(6) 0.050(6) 0.002(5) -0.008(6) -0.010(5)
C29A 0.035(5) 0.034(5) 0.056(6) 0.006(5) -0.009(5) -0.006(5)
C30 0.054(11) 0.042(11) 0.048(9) 0.003(9) -0.010(9) -0.017(9)
C30A 0.047(10) 0.041(10) 0.058(8) 0.005(8) -0.012(8) -0.011(8)
C31 0.037(9) 0.036(8) 0.078(13) -0.005(9) -0.008(9) -0.010(7)
C31A 0.042(9) 0.029(7) 0.065(10) 0.003(8) -0.003(9) -0.004(7)
C32 0.039(7) 0.045(8) 0.062(9) 0.009(7) -0.006(6) -0.009(6)
C33 0.042(7) 0.043(8) 0.053(8) 0.016(6) -0.006(6) 0.003(6)
N4 0.040(6) 0.045(6) 0.040(6) -0.005(5) -0.010(5) -0.011(5)
_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
U1 Te1 3.0807(4) . ?
U1 N1 2.225(9) . ?
U1 N2 2.205(10) . ?
U1 N3 2.211(10) . ?
U1 N4 2.709(12) . ?
N1 Si1 1.767(10) . ?
N1 Si1A 1.799(9) . ?
N1 C10 1.50(2) . ?
Si1 C1 1.898(15) . ?
Si1 C4 1.909(14) . ?
Si1 C7 1.894(14) . ?
Si1A C1A 1.903(14) . ?
Si1A C4A 1.914(13) . ?
Si1A C7A 1.902(14) . ?
C1 H1 0.9800 . ?
C1 C2 1.516(15) . ?
C1 C3 1.519(15) . ?
C1A H1A 0.9800 . ?
C1A C2A 1.526(15) . ?
C1A C3A 1.520(15) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C2A H2AA 0.9600 . ?
C2A H2AB 0.9600 . ?
C2A H2AC 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C3A H3AA 0.9600 . ?
C3A H3AB 0.9600 . ?
C3A H3AC 0.9600 . ?
C4 H4 0.9800 . ?
C4 C5 1.522(15) . ?
C4 C6 1.519(15) . ?
C4A H4A 0.9800 . ?
C4A C5A 1.523(15) . ?
C4A C6A 1.528(14) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C5A H5AA 0.9600 . ?
C5A H5AB 0.9600 . ?
C5A H5AC 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
C6A H6AA 0.9600 . ?
C6A H6AB 0.9600 . ?
C6A H6AC 0.9600 . ?
C7 H7 0.9800 . ?
C7 C8 1.519(15) . ?
C7 C9 1.511(15) . ?
C7A H7A 0.9800 . ?
C7A C8A 1.514(15) . ?
C7A C9A 1.522(15) . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C8A H8AA 0.9600 . ?
C8A H8AB 0.9600 . ?
C8A H8AC 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C9A H9AA 0.9600 . ?
C9A H9AB 0.9600 . ?
C9A H9AC 0.9600 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C10 C11 1.53(2) . ?
C11 H11A 0.9700 . ?
C11 H11B 0.9700 . ?
C11 N4 1.493(17) . ?
N2 Si2 1.821(10) . ?
N2 Si2A 1.734(9) . ?
N2 C21 1.54(2) . ?
Si2 C12 1.899(14) . ?
Si2 C15 1.910(14) . ?
Si2 C18 1.913(14) . ?
Si2A C12A 1.896(15) . ?
Si2A C15A 1.898(14) . ?
Si2A C18A 1.892(14) . ?
C12 H12 0.9800 . ?
C12 C13 1.523(15) . ?
C12 C14 1.528(15) . ?
C12A H12A 0.9800 . ?
C12A C13A 1.520(15) . ?
C12A C14A 1.516(15) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C13A H13D 0.9600 . ?
C13A H13E 0.9600 . ?
C13A H13F 0.9600 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C14A H14D 0.9600 . ?
C14A H14E 0.9600 . ?
C14A H14F 0.9600 . ?
C15 H15 0.9800 . ?
C15 C16 1.523(15) . ?
C15 C17 1.527(15) . ?
C15A H15A 0.9800 . ?
C15A C16A 1.515(15) . ?
C15A C17A 1.521(15) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C16A H16D 0.9600 . ?
C16A H16E 0.9600 . ?
C16A H16F 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C17A H17D 0.9600 . ?
C17A H17E 0.9600 . ?
C17A H17F 0.9600 . ?
C18 H18 0.9800 . ?
C18 C19 1.522(15) . ?
C18 C20 1.523(15) . ?
C18A H18A 0.9800 . ?
C18A C19A 1.522(15) . ?
C18A C20A 1.521(15) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C19A H19D 0.9600 . ?
C19A H19E 0.9600 . ?
C19A H19F 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C20A H20D 0.9600 . ?
C20A H20E 0.9600 . ?
C20A H20F 0.9600 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C21 C22 1.47(3) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C22 N4 1.49(2) . ?
N3 Si3 1.763(9) . ?
N3 Si3A 1.807(10) . ?
N3 C32 1.506(19) . ?
Si3 C23 1.898(14) . ?
Si3 C26 1.900(14) . ?
Si3 C29 1.887(14) . ?
Si3A C23A 1.910(14) . ?
Si3A C26A 1.909(14) . ?
Si3A C29A 1.904(14) . ?
C23 H23 0.9800 . ?
C23 C24 1.525(15) . ?
C23 C25 1.522(15) . ?
C23A H23A 0.9800 . ?
C23A C24A 1.518(15) . ?
C23A C25A 1.528(15) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C24A H24D 0.9600 . ?
C24A H24E 0.9600 . ?
C24A H24F 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C25A H25D 0.9600 . ?
C25A H25E 0.9600 . ?
C25A H25F 0.9600 . ?
C26 H26 0.9800 . ?
C26 C27 1.514(15) . ?
C26 C28 1.521(15) . ?
C26A H26A 0.9800 . ?
C26A C27A 1.529(15) . ?
C26A C28A 1.521(15) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C27A H27D 0.9600 . ?
C27A H27E 0.9600 . ?
C27A H27F 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C28A H28D 0.9600 . ?
C28A H28E 0.9600 . ?
C28A H28F 0.9600 . ?
C29 H29 0.9800 . ?
C29 C30 1.518(15) . ?
C29 C31 1.520(15) . ?
C29A H29A 0.9800 . ?
C29A C30A 1.516(15) . ?
C29A C31A 1.516(15) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C30A H30D 0.9600 . ?
C30A H30E 0.9600 . ?
C30A H30F 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C31A H31D 0.9600 . ?
C31A H31E 0.9600 . ?
C31A H31F 0.9600 . ?
C32 H32A 0.9700 . ?
C32 H32B 0.9700 . ?
C32 C33 1.54(2) . ?
C33 H33A 0.9700 . ?
C33 H33B 0.9700 . ?
C33 N4 1.483(18) . ?
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
N1 U1 Te1 111.4(3) . . ?
N1 U1 N4 69.5(3) . . ?
N2 U1 Te1 107.4(3) . . ?
N2 U1 N1 109.4(4) . . ?
N2 U1 N3 108.0(4) . . ?
N2 U1 N4 70.2(4) . . ?
N3 U1 Te1 112.4(3) . . ?
N3 U1 N1 108.2(4) . . ?
N3 U1 N4 69.1(4) . . ?
N4 U1 Te1 177.5(3) . . ?
U1 Te1 U1 180.0 . 3_575 ?
Si1 N1 U1 143.0(7) . . ?
Si1A N1 U1 131.4(7) . . ?
C10 N1 U1 111.8(8) . . ?
C10 N1 Si1 104.9(9) . . ?
C10 N1 Si1A 116.3(9) . . ?
N1 Si1 C1 99.3(9) . . ?
N1 Si1 C4 111.1(9) . . ?
N1 Si1 C7 114.3(12) . . ?
C1 Si1 C4 116.7(14) . . ?
C7 Si1 C1 109.9(12) . . ?
C7 Si1 C4 105.8(11) . . ?
N1 Si1A C1A 113.7(8) . . ?
N1 Si1A C4A 110.0(8) . . ?
N1 Si1A C7A 108.6(10) . . ?
C1A Si1A C4A 110.7(11) . . ?
C7A Si1A C1A 107.1(10) . . ?
C7A Si1A C4A 106.3(9) . . ?
Si1 C1 H1 106.8 . . ?
C2 C1 Si1 113.4(18) . . ?
C2 C1 H1 106.8 . . ?
C2 C1 C3 107(2) . . ?
C3 C1 Si1 115.5(17) . . ?
C3 C1 H1 106.8 . . ?
Si1A C1A H1A 105.9 . . ?
C2A C1A Si1A 112.0(15) . . ?
C2A C1A H1A 105.9 . . ?
C3A C1A Si1A 114.6(14) . . ?
C3A C1A H1A 105.9 . . ?
C3A C1A C2A 111.7(19) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1A C2A H2AA 109.5 . . ?
C1A C2A H2AB 109.5 . . ?
C1A C2A H2AC 109.5 . . ?
H2AA C2A H2AB 109.5 . . ?
H2AA C2A H2AC 109.5 . . ?
H2AB C2A H2AC 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1A C3A H3AA 109.5 . . ?
C1A C3A H3AB 109.5 . . ?
C1A C3A H3AC 109.5 . . ?
H3AA C3A H3AB 109.5 . . ?
H3AA C3A H3AC 109.5 . . ?
H3AB C3A H3AC 109.5 . . ?
Si1 C4 H4 106.5 . . ?
C5 C4 Si1 115.3(17) . . ?
C5 C4 H4 106.5 . . ?
C6 C4 Si1 111.9(18) . . ?
C6 C4 H4 106.5 . . ?
C6 C4 C5 109(2) . . ?
Si1A C4A H4A 105.2 . . ?
C5A C4A Si1A 115.4(15) . . ?
C5A C4A H4A 105.2 . . ?
C5A C4A C6A 108.4(18) . . ?
C6A C4A Si1A 116.4(15) . . ?
C6A C4A H4A 105.2 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
C4A C5A H5AA 109.5 . . ?
C4A C5A H5AB 109.5 . . ?
C4A C5A H5AC 109.5 . . ?
H5AA C5A H5AB 109.5 . . ?
H5AA C5A H5AC 109.5 . . ?
H5AB C5A H5AC 109.5 . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4A C6A H6AA 109.5 . . ?
C4A C6A H6AB 109.5 . . ?
C4A C6A H6AC 109.5 . . ?
H6AA C6A H6AB 109.5 . . ?
H6AA C6A H6AC 109.5 . . ?
H6AB C6A H6AC 109.5 . . ?
Si1 C7 H7 105.1 . . ?
C8 C7 Si1 111.7(17) . . ?
C8 C7 H7 105.1 . . ?
C9 C7 Si1 118.4(19) . . ?
C9 C7 H7 105.1 . . ?
C9 C7 C8 110(3) . . ?
Si1A C7A H7A 105.1 . . ?
C8A C7A Si1A 111.9(15) . . ?
C8A C7A H7A 105.1 . . ?
C8A C7A C9A 115(2) . . ?
C9A C7A Si1A 113.7(15) . . ?
C9A C7A H7A 105.1 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7A C8A H8AA 109.5 . . ?
C7A C8A H8AB 109.5 . . ?
C7A C8A H8AC 109.5 . . ?
H8AA C8A H8AB 109.5 . . ?
H8AA C8A H8AC 109.5 . . ?
H8AB C8A H8AC 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7A C9A H9AA 109.5 . . ?
C7A C9A H9AB 109.5 . . ?
C7A C9A H9AC 109.5 . . ?
H9AA C9A H9AB 109.5 . . ?
H9AA C9A H9AC 109.5 . . ?
H9AB C9A H9AC 109.5 . . ?
N1 C10 H10A 110.0 . . ?
N1 C10 H10B 110.0 . . ?
N1 C10 C11 108.3(13) . . ?
H10A C10 H10B 108.4 . . ?
C11 C10 H10A 110.0 . . ?
C11 C10 H10B 110.0 . . ?
C10 C11 H11A 110.1 . . ?
C10 C11 H11B 110.1 . . ?
H11A C11 H11B 108.4 . . ?
N4 C11 C10 108.1(11) . . ?
N4 C11 H11A 110.1 . . ?
N4 C11 H11B 110.1 . . ?
Si2 N2 U1 127.7(7) . . ?
Si2A N2 U1 148.1(8) . . ?
C21 N2 U1 109.1(8) . . ?
C21 N2 Si2 123.2(9) . . ?
C21 N2 Si2A 101.5(10) . . ?
N2 Si2 C12 114.1(9) . . ?
N2 Si2 C15 108.2(9) . . ?
N2 Si2 C18 109.6(8) . . ?
C12 Si2 C15 109.5(12) . . ?
C12 Si2 C18 105.9(10) . . ?
C15 Si2 C18 109.6(10) . . ?
N2 Si2A C12A 99.1(9) . . ?
N2 Si2A C15A 112.4(9) . . ?
N2 Si2A C18A 114.1(11) . . ?
C12A Si2A C15A 114.5(12) . . ?
C18A Si2A C12A 107.6(11) . . ?
C18A Si2A C15A 109.0(10) . . ?
Si2 C12 H12 106.0 . . ?
C13 C12 Si2 115.8(17) . . ?
C13 C12 H12 106.0 . . ?
C13 C12 C14 107(2) . . ?
C14 C12 Si2 115.4(16) . . ?
C14 C12 H12 106.0 . . ?
Si2A C12A H12A 106.8 . . ?
C13A C12A Si2A 112.4(18) . . ?
C13A C12A H12A 106.8 . . ?
C14A C12A Si2A 113.3(16) . . ?
C14A C12A H12A 106.8 . . ?
C14A C12A C13A 110(2) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12A C13A H13D 109.5 . . ?
C12A C13A H13E 109.5 . . ?
C12A C13A H13F 109.5 . . ?
H13D C13A H13E 109.5 . . ?
H13D C13A H13F 109.5 . . ?
H13E C13A H13F 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12A C14A H14D 109.5 . . ?
C12A C14A H14E 109.5 . . ?
C12A C14A H14F 109.5 . . ?
H14D C14A H14E 109.5 . . ?
H14D C14A H14F 109.5 . . ?
H14E C14A H14F 109.5 . . ?
Si2 C15 H15 104.8 . . ?
C16 C15 Si2 118.4(15) . . ?
C16 C15 H15 104.8 . . ?
C16 C15 C17 110(2) . . ?
C17 C15 Si2 112.2(16) . . ?
C17 C15 H15 104.8 . . ?
Si2A C15A H15A 106.4 . . ?
C16A C15A Si2A 112.2(16) . . ?
C16A C15A H15A 106.4 . . ?
C16A C15A C17A 109(2) . . ?
C17A C15A Si2A 115.8(18) . . ?
C17A C15A H15A 106.4 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C15A C16A H16D 109.5 . . ?
C15A C16A H16E 109.5 . . ?
C15A C16A H16F 109.5 . . ?
H16D C16A H16E 109.5 . . ?
H16D C16A H16F 109.5 . . ?
H16E C16A H16F 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15A C17A H17D 109.5 . . ?
C15A C17A H17E 109.5 . . ?
C15A C17A H17F 109.5 . . ?
H17D C17A H17E 109.5 . . ?
H17D C17A H17F 109.5 . . ?
H17E C17A H17F 109.5 . . ?
Si2 C18 H18 105.0 . . ?
C19 C18 Si2 117.7(15) . . ?
C19 C18 H18 105.0 . . ?
C19 C18 C20 110(2) . . ?
C20 C18 Si2 112.7(16) . . ?
C20 C18 H18 105.0 . . ?
Si2A C18A H18A 106.6 . . ?
C19A C18A Si2A 111.7(16) . . ?
C19A C18A H18A 106.6 . . ?
C20A C18A Si2A 113.4(17) . . ?
C20A C18A H18A 106.6 . . ?
C20A C18A C19A 111(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
H19D C19A H19E 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18A C20A H20D 109.5 . . ?
C18A C20A H20E 109.5 . . ?
C18A C20A H20F 109.5 . . ?
H20D C20A H20E 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
N2 C21 H21A 109.8 . . ?
N2 C21 H21B 109.8 . . ?
H21A C21 H21B 108.2 . . ?
C22 C21 N2 109.4(11) . . ?
C22 C21 H21A 109.8 . . ?
C22 C21 H21B 109.8 . . ?
C21 C22 H22A 110.1 . . ?
C21 C22 H22B 110.1 . . ?
C21 C22 N4 108.2(11) . . ?
H22A C22 H22B 108.4 . . ?
N4 C22 H22A 110.1 . . ?
N4 C22 H22B 110.1 . . ?
Si3 N3 U1 138.3(7) . . ?
Si3A N3 U1 132.7(7) . . ?
C32 N3 U1 111.1(8) . . ?
C32 N3 Si3 109.1(9) . . ?
C32 N3 Si3A 114.8(9) . . ?
N3 Si3 C23 101.4(8) . . ?
N3 Si3 C26 108.7(9) . . ?
N3 Si3 C29 118.4(10) . . ?
C23 Si3 C26 115.4(13) . . ?
C29 Si3 C23 108.0(10) . . ?
C29 Si3 C26 105.4(10) . . ?
N3 Si3A C23A 113.4(9) . . ?
N3 Si3A C26A 112.7(10) . . ?
N3 Si3A C29A 110.8(10) . . ?
C26A Si3A C23A 110.8(14) . . ?
C29A Si3A C23A 103.4(11) . . ?
C29A Si3A C26A 105.0(10) . . ?
Si3 C23 H23 107.0 . . ?
C24 C23 Si3 113.5(16) . . ?
C24 C23 H23 107.0 . . ?
C25 C23 Si3 113.0(16) . . ?
C25 C23 H23 107.0 . . ?
C25 C23 C24 109(2) . . ?
Si3A C23A H23A 106.0 . . ?
C24A C23A Si3A 116.2(16) . . ?
C24A C23A H23A 106.0 . . ?
C24A C23A C25A 107(2) . . ?
C25A C23A Si3A 114.8(19) . . ?
C25A C23A H23A 106.0 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23A C24A H24D 109.5 . . ?
C23A C24A H24E 109.5 . . ?
C23A C24A H24F 109.5 . . ?
H24D C24A H24E 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C23A C25A H25D 109.5 . . ?
C23A C25A H25E 109.5 . . ?
C23A C25A H25F 109.5 . . ?
H25D C25A H25E 109.5 . . ?
H25D C25A H25F 109.5 . . ?
H25E C25A H25F 109.5 . . ?
Si3 C26 H26 106.3 . . ?
C27 C26 Si3 115.1(17) . . ?
C27 C26 H26 106.3 . . ?
C27 C26 C28 108(2) . . ?
C28 C26 Si3 114.2(17) . . ?
C28 C26 H26 106.3 . . ?
Si3A C26A H26A 106.1 . . ?
C27A C26A Si3A 114.5(18) . . ?
C27A C26A H26A 106.1 . . ?
C28A C26A Si3A 116.1(17) . . ?
C28A C26A H26A 106.1 . . ?
C28A C26A C27A 107(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26A C27A H27D 109.5 . . ?
C26A C27A H27E 109.5 . . ?
C26A C27A H27F 109.5 . . ?
H27D C27A H27E 109.5 . . ?
H27D C27A H27F 109.5 . . ?
H27E C27A H27F 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26A C28A H28D 109.5 . . ?
C26A C28A H28E 109.5 . . ?
C26A C28A H28F 109.5 . . ?
H28D C28A H28E 109.5 . . ?
H28D C28A H28F 109.5 . . ?
H28E C28A H28F 109.5 . . ?
Si3 C29 H29 106.1 . . ?
C30 C29 Si3 117.5(17) . . ?
C30 C29 H29 106.1 . . ?
C30 C29 C31 111(2) . . ?
C31 C29 Si3 109.8(15) . . ?
C31 C29 H29 106.1 . . ?
Si3A C29A H29A 108.3 . . ?
C30A C29A Si3A 111.5(16) . . ?
C30A C29A H29A 108.3 . . ?
C30A C29A C31A 108(2) . . ?
C31A C29A Si3A 112.0(15) . . ?
C31A C29A H29A 108.3 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29A C30A H30D 109.5 . . ?
C29A C30A H30E 109.5 . . ?
C29A C30A H30F 109.5 . . ?
H30D C30A H30E 109.5 . . ?
H30D C30A H30F 109.5 . . ?
H30E C30A H30F 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29A C31A H31D 109.5 . . ?
C29A C31A H31E 109.5 . . ?
C29A C31A H31F 109.5 . . ?
H31D C31A H31E 109.5 . . ?
H31D C31A H31F 109.5 . . ?
H31E C31A H31F 109.5 . . ?
N3 C32 H32A 110.2 . . ?
N3 C32 H32B 110.2 . . ?
N3 C32 C33 107.7(13) . . ?
H32A C32 H32B 108.5 . . ?
C33 C32 H32A 110.2 . . ?
C33 C32 H32B 110.2 . . ?
C32 C33 H33A 110.4 . . ?
C32 C33 H33B 110.4 . . ?
H33A C33 H33B 108.6 . . ?
N4 C33 C32 106.5(11) . . ?
N4 C33 H33A 110.4 . . ?
N4 C33 H33B 110.4 . . ?
C11 N4 U1 106.9(7) . . ?
C22 N4 U1 105.8(9) . . ?
C22 N4 C11 111.9(12) . . ?
C33 N4 U1 107.6(8) . . ?
C33 N4 C11 111.9(13) . . ?
C33 N4 C22 112.4(11) . . ?
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
U1 N1 Si1 C1 -12.6(16) . . . . ?
U1 N1 Si1 C4 -136.0(14) . . . . ?
U1 N1 Si1 C7 104.4(14) . . . . ?
U1 N1 Si1A C1A -2.0(13) . . . . ?
U1 N1 Si1A C4A -126.9(10) . . . . ?
U1 N1 Si1A C7A 117.1(10) . . . . ?
U1 N1 C10 C11 67.2(14) . . . . ?
U1 N2 Si2 C12 -23.2(12) . . . . ?
U1 N2 Si2 C15 -145.4(9) . . . . ?
U1 N2 Si2 C18 95.2(11) . . . . ?
U1 N2 Si2A C12A -24.9(16) . . . . ?
U1 N2 Si2A C15A -146.2(14) . . . . ?
U1 N2 Si2A C18A 89.1(16) . . . . ?
U1 N2 C21 C22 69.0(12) . . . . ?
U1 N3 Si3 C23 -13.9(15) . . . . ?
U1 N3 Si3 C26 -135.9(13) . . . . ?
U1 N3 Si3 C29 104.0(13) . . . . ?
U1 N3 Si3A C23A 1.1(14) . . . . ?
U1 N3 Si3A C26A -125.8(12) . . . . ?
U1 N3 Si3A C29A 116.9(11) . . . . ?
U1 N3 C32 C33 69.5(13) . . . . ?
N1 Si1 C1 C2 176(2) . . . . ?
N1 Si1 C1 C3 -60(2) . . . . ?
N1 Si1 C7 C8 -55(3) . . . . ?
N1 Si1 C7 C9 74(3) . . . . ?
N1 C10 C11 N4 -59.7(17) . . . . ?
Si1 N1 C10 C11 -117.7(12) . . . . ?
Si1A N1 C10 C11 -105.0(12) . . . . ?
C1 Si1 C7 C8 55(3) . . . . ?
C1 Si1 C7 C9 -175(2) . . . . ?
C4 Si1 C1 C2 -64(2) . . . . ?
C4 Si1 C1 C3 60(2) . . . . ?
C4 Si1 C7 C8 -178(2) . . . . ?
C4 Si1 C7 C9 -48(3) . . . . ?
C7 Si1 C1 C2 56(2) . . . . ?
C7 Si1 C1 C3 -180(2) . . . . ?
C10 N1 Si1 C1 175.0(12) . . . . ?
C10 N1 Si1 C4 51.5(15) . . . . ?
C10 N1 Si1 C7 -68.1(13) . . . . ?
C10 N1 Si1A C1A 168.4(12) . . . . ?
C10 N1 Si1A C4A 43.5(14) . . . . ?
C10 N1 Si1A C7A -72.5(13) . . . . ?
C10 C11 N4 U1 26.6(15) . . . . ?
C10 C11 N4 C22 141.9(14) . . . . ?
C10 C11 N4 C33 -90.9(15) . . . . ?
N2 Si2 C12 C13 -157.2(18) . . . . ?
N2 Si2 C12 C14 -31(2) . . . . ?
N2 Si2A C12A C13A -176.8(18) . . . . ?
N2 Si2A C12A C14A -51(2) . . . . ?
N2 Si2A C15A C16A -167.5(18) . . . . ?
N2 Si2A C15A C17A 66(3) . . . . ?
N2 Si2A C18A C19A -70(2) . . . . ?
N2 Si2A C18A C20A 57(2) . . . . ?
N2 C21 C22 N4 -61.7(16) . . . . ?
Si2 N2 C21 C22 -112.6(13) . . . . ?
Si2A N2 C21 C22 -120.4(11) . . . . ?
C12A Si2A C15A C16A 81(2) . . . . ?
C12A Si2A C15A C17A -46(3) . . . . ?
C12A Si2A C18A C19A 38(2) . . . . ?
C12A Si2A C18A C20A 165.4(19) . . . . ?
C15 Si2 C12 C13 -36(2) . . . . ?
C15 Si2 C12 C14 90.2(19) . . . . ?
C15A Si2A C12A C13A -57(2) . . . . ?
C15A Si2A C12A C14A 69(2) . . . . ?
C15A Si2A C18A C19A 163(2) . . . . ?
C15A Si2A C18A C20A -70(2) . . . . ?
C18 Si2 C12 C13 82(2) . . . . ?
C18 Si2 C12 C14 -151.8(18) . . . . ?
C18A Si2A C12A C13A 64(2) . . . . ?
C18A Si2A C12A C14A -169.8(19) . . . . ?
C18A Si2A C15A C16A -40(2) . . . . ?
C18A Si2A C15A C17A -166(2) . . . . ?
C21 N2 Si2 C12 158.7(12) . . . . ?
C21 N2 Si2 C15 36.5(13) . . . . ?
C21 N2 Si2 C18 -82.8(13) . . . . ?
C21 N2 Si2A C12A 172.1(10) . . . . ?
C21 N2 Si2A C15A 50.8(13) . . . . ?
C21 N2 Si2A C18A -73.9(11) . . . . ?
C21 C22 N4 U1 26.7(14) . . . . ?
C21 C22 N4 C11 -89.3(16) . . . . ?
C21 C22 N4 C33 143.8(13) . . . . ?
N3 Si3 C23 C24 -52(2) . . . . ?
N3 Si3 C23 C25 -177(2) . . . . ?
N3 Si3 C26 C27 63(2) . . . . ?
N3 Si3 C26 C28 -171(2) . . . . ?
N3 Si3 C29 C30 71(2) . . . . ?
N3 Si3 C29 C31 -56(2) . . . . ?
N3 C32 C33 N4 -60.9(15) . . . . ?
Si3 N3 C32 C33 -121.8(11) . . . . ?
Si3A N3 C32 C33 -99.1(12) . . . . ?
C23 Si3 C26 C27 -50(2) . . . . ?
C23 Si3 C26 C28 76(2) . . . . ?
C23 Si3 C29 C30 -174(2) . . . . ?
C23 Si3 C29 C31 58(2) . . . . ?
C26 Si3 C23 C24 65(2) . . . . ?
C26 Si3 C23 C25 -60(2) . . . . ?
C26 Si3 C29 C30 -51(2) . . . . ?
C26 Si3 C29 C31 -178(2) . . . . ?
C29 Si3 C23 C24 -178(2) . . . . ?
C29 Si3 C23 C25 58(2) . . . . ?
C29 Si3 C26 C27 -169(2) . . . . ?
C29 Si3 C26 C28 -43(3) . . . . ?
C32 N3 Si3 C23 -177.9(12) . . . . ?
C32 N3 Si3 C26 60.0(14) . . . . ?
C32 N3 Si3 C29 -60.1(14) . . . . ?
C32 N3 Si3A C23A 166.6(13) . . . . ?
C32 N3 Si3A C26A 39.6(15) . . . . ?
C32 N3 Si3A C29A -77.6(13) . . . . ?
C32 C33 N4 U1 27.0(14) . . . . ?
C32 C33 N4 C11 144.0(13) . . . . ?
C32 C33 N4 C22 -89.1(15) . . . . ?
_shelx_res_file
;
TITL UBMGNF in P21/n #14
ubmgnf.res
created by SHELXL-2016/6 at 16:38:43 on 27-Apr-2017
REM reset to P21/n #14
CELL 1.54184 13.802162 16.375096 18.098539 90 92.4744 90
ZERR 2 0.000332 0.000454 0.000581 0 0.0025 0
LATT 1
SYMM 0.5-X,0.5+Y,0.5-Z
SFAC C H N Si Te U
UNIT 132 300 16 12 2 4
SADI 0.01 Si2 N2 Si2A N2 Si1 N1 Si1A N1 Si3A N3 Si3 N3
SADI Si3A C29A Si3 C29 Si3 C23 Si3A C23A Si3 C26 Si3A C26A Si1 C4 Si1A C4A =
SI1 C1 SI1A C1A SI1A C7A SI1 C7 SI2 C18 SI2 C12 SI2A C12A SI2A C18A SI2A =
C15A SI2 C15
SADI C19A C18A C20A C18A C19 C18 C20 C18 C13 C12 C14 C12 C13A C12A C14A C12A =
C16 C15 C17 C15 C17A C15A C16A C15A C31 C29 C30 C29 C30A C29A C31A C29A C28 =
C26 C27 C26 C28A C26A C27A C26A C24A C23A C25A C23A C25 C23 C24 C23 C8A C7A =
C8 C7 C9 C7 C9A C7A C5A C4A C5 C4 C6A C4A C6 C4 C2 C1 C2A C1A C3 C1 C3A C1A
SIMU 0.01 0.02 2 Si1 Si1A C1 C2 C2A C4 C4A C5 C5A C6 C6A C7 C7A C8 C8A C9 =
C9A C1A C3 C3A SI2 C12 C12A C13 C13A C14 C14A C15 C15A C16 C16A C17 C17A C18 =
C19 C18A C19A C20 C20A SI2A SI3 SI3A C23 C23A C24 C24A C25 C25A C26 C26A C27 =
C27A C28 C28A C29 C29A C30 C30A C31 C31A
RIGU Si2 Si2A C12 C12A C13 C13A C14 C14A C15 C15A C16 C16A C17 C17A C18 C18A =
C19 C19A C20 C20A SI3 C25 C26 C26A C28 C28A C29 C29A C30 C30A C31 C31A SI3A =
C23 C23A C24 C24A C25A C27 C27A SI1 SI1A C1 C1A C2 C2A C3 C3A C4 C4A C5 C5A =
C6 C6A C7 C7A C8 C8A C9 C9A N2
L.S. 16
PLAN 20
BOND $H
CONF
temp
MORE -1
fmap 2
acta
OMIT -3 2 3
OMIT -10 0 14
REM
REM
REM
WGHT 0.113800 64.730095
FVAR 1.56758 0.49895 0.44836 0.51550
U1 6 0.060589 0.851966 0.096356 11.00000 0.02673 0.03109 =
0.02719 0.00171 -0.00697 -0.00130
TE1 5 0.000000 1.000000 0.000000 10.50000 0.03895 0.02836 =
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N1 3 0.021517 0.734970 0.040151 11.00000 0.06424 0.01423 =
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PART 1
SI1 4 -0.059494 0.690951 -0.026827 31.00000 0.05709 0.02329 =
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PART 0
PART 2
SI1A 4 -0.086099 0.704110 -0.012210 -31.00000 0.06015 0.02871 =
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PART 0
PART 1
C1 1 -0.150447 0.777515 -0.037656 31.00000 0.05522 0.03054 =
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AFIX 13
H1 2 -0.114525 0.825576 -0.053563 31.00000 -1.20000
AFIX 0
PART 0
PART 2
C1A 1 -0.184535 0.785545 -0.017634 -31.00000 0.05191 0.03466 =
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AFIX 13
H1A 2 -0.159381 0.829515 -0.048143 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C2 1 -0.229583 0.761631 -0.096601 31.00000 0.06495 0.05005 =
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AFIX 137
H2A 2 -0.201091 0.741746 -0.140592 31.00000 -1.50000
H2B 2 -0.263893 0.811475 -0.107546 31.00000 -1.50000
H2C 2 -0.273878 0.721612 -0.078992 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C2A 1 -0.276561 0.755131 -0.058513 -31.00000 0.06036 0.04219 =
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AFIX 137
H2AA 2 -0.260010 0.730124 -0.104257 -31.00000 -1.50000
H2AB 2 -0.319417 0.800338 -0.068551 -31.00000 -1.50000
H2AC 2 -0.308162 0.715795 -0.028455 -31.00000 -1.50000
AFIX 0
PART 0
PART 1
C3 1 -0.200472 0.801669 0.032207 31.00000 0.04308 0.04717 =
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AFIX 137
H3A 2 -0.234970 0.755533 0.050570 31.00000 -1.50000
H3B 2 -0.245229 0.845330 0.021236 31.00000 -1.50000
H3C 2 -0.152832 0.819411 0.068967 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C3A 1 -0.206301 0.824494 0.056061 -31.00000 0.03252 0.04591 =
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AFIX 137
H3AA 2 -0.212209 0.782654 0.092747 -31.00000 -1.50000
H3AB 2 -0.265934 0.854559 0.051045 -31.00000 -1.50000
H3AC 2 -0.154508 0.860867 0.070931 -31.00000 -1.50000
AFIX 0
PART 0
PART 1
C4 1 -0.107784 0.588750 0.006471 31.00000 0.05790 0.02660 =
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AFIX 13
H4 2 -0.051183 0.553526 0.015861 31.00000 -1.20000
AFIX 0
PART 0
PART 2
C4A 1 -0.135112 0.604334 0.026710 -31.00000 0.05496 0.03137 =
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AFIX 13
H4A 2 -0.077524 0.572713 0.042331 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C5 1 -0.161193 0.591946 0.078220 31.00000 0.06017 0.03399 =
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AFIX 137
H5A 2 -0.127301 0.627613 0.112583 31.00000 -1.50000
H5B 2 -0.164216 0.538106 0.098984 31.00000 -1.50000
H5C 2 -0.225761 0.612136 0.068364 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C5A 1 -0.193184 0.613175 0.095929 -31.00000 0.05640 0.04446 =
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AFIX 137
H5AA 2 -0.252941 0.641046 0.083723 -31.00000 -1.50000
H5AB 2 -0.156274 0.644015 0.132417 -31.00000 -1.50000
H5AC 2 -0.206944 0.560037 0.115279 -31.00000 -1.50000
AFIX 0
PART 0
PART 1
C6 1 -0.171020 0.546571 -0.052784 31.00000 0.05277 0.03747 =
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AFIX 137
H6A 2 -0.228441 0.578419 -0.063000 31.00000 -1.50000
H6B 2 -0.188899 0.493375 -0.035726 31.00000 -1.50000
H6C 2 -0.135680 0.541269 -0.097068 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C6A 1 -0.191835 0.549372 -0.027908 -31.00000 0.05865 0.03666 =
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AFIX 137
H6AA 2 -0.258941 0.564976 -0.029828 -31.00000 -1.50000
H6AB 2 -0.185942 0.493569 -0.012085 -31.00000 -1.50000
H6AC 2 -0.166269 0.555027 -0.076137 -31.00000 -1.50000
AFIX 0
PART 0
PART 1
C7 1 -0.004032 0.669127 -0.118690 31.00000 0.05757 0.02953 =
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AFIX 13
H7 2 -0.059055 0.655975 -0.152640 31.00000 -1.20000
AFIX 0
PART 0
PART 2
C7A 1 -0.052292 0.681066 -0.110848 -31.00000 0.06125 0.03311 =
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AFIX 13
H7A 2 -0.109058 0.653386 -0.133555 -31.00000 -1.20000
AFIX 0
PART 0
PART 1
C8 1 0.041184 0.745140 -0.150806 31.00000 0.07647 0.03991 =
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AFIX 137
H8A 2 -0.006371 0.787892 -0.154517 31.00000 -1.50000
H8B 2 0.063643 0.733055 -0.199069 31.00000 -1.50000
H8C 2 0.094852 0.762508 -0.119128 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C8A 1 -0.040834 0.758247 -0.155725 -31.00000 0.07184 0.03807 =
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AFIX 137
H8AA 2 -0.100439 0.788525 -0.156866 -31.00000 -1.50000
H8AB 2 -0.025020 0.744144 -0.205260 -31.00000 -1.50000
H8AC 2 0.010223 0.791002 -0.133499 -31.00000 -1.50000
AFIX 0
PART 0
PART 1
C9 1 0.064229 0.597424 -0.123672 31.00000 0.05651 0.04219 =
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AFIX 137
H9A 2 0.123334 0.608980 -0.095719 31.00000 -1.50000
H9B 2 0.078316 0.588107 -0.174466 31.00000 -1.50000
H9C 2 0.034419 0.549616 -0.103998 31.00000 -1.50000
AFIX 0
PART 0
PART 2
C9A 1 0.030553 0.620229 -0.115885 -31.00000 0.06667 0.04036 =
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AFIX 137
H9AA 2 0.088900 0.643637 -0.094247 -31.00000 -1.50000
H9AB 2 0.039947 0.607433 -0.166843 -31.00000 -1.50000
H9AC 2 0.015058 0.571251 -0.089742 -31.00000 -1.50000
AFIX 0
PART 0
C10 1 0.093525 0.668896 0.059253 11.00000 0.07096 0.04648 =
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AFIX 23
H10A 2 0.158574 0.687432 0.049779 11.00000 -1.20000
H10B 2 0.079695 0.620910 0.029193 11.00000 -1.20000
AFIX 0
C11 1 0.086077 0.648002 0.141212 11.00000 0.08812 0.02260 =
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AFIX 23
H11A 2 0.021334 0.628635 0.150577 11.00000 -1.20000
H11B 2 0.132045 0.605334 0.155197 11.00000 -1.20000
AFIX 0
N2 3 -0.016769 0.861206 0.200087 11.00000 0.03378 0.08867 =
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PART 1
SI2 4 -0.049274 0.953635 0.249152 41.00000 0.02923 0.05721 =
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PART 0
PART 2
SI2A 4 -0.080370 0.921585 0.260042 -41.00000 0.02703 0.05245 =
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PART 0
PART 1
C12 1 0.028836 1.045587 0.228335 41.00000 0.03486 0.05442 =
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AFIX 13
H12 2 -0.000725 1.070573 0.183616 41.00000 -1.20000
AFIX 0
PART 0
PART 2
C12A 1 -0.029611 1.025090 0.234997 -41.00000 0.03576 0.05352 =
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AFIX 13
H12A 2 -0.052284 1.036429 0.183968 -41.00000 -1.20000
AFIX 0
PART 0
PART 1
C13 1 0.032626 1.112434 0.286893 41.00000 0.05122 0.05146 =
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AFIX 137
H13A 2 -0.032141 1.126563 0.299429 41.00000 -1.50000
H13B 2 0.064310 1.159719 0.267924 41.00000 -1.50000
H13C 2 0.068097 1.093158 0.330239 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C13A 1 -0.067951 1.093432 0.282460 -41.00000 0.05470 0.05442 =
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AFIX 137
H13D 2 -0.043371 1.086839 0.332537 -41.00000 -1.50000
H13E 2 -0.137523 1.091506 0.281072 -41.00000 -1.50000
H13F 2 -0.047180 1.145120 0.263754 -41.00000 -1.50000
AFIX 0
PART 0
PART 1
C14 1 0.133630 1.026364 0.210458 41.00000 0.03572 0.03258 =
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AFIX 137
H14A 2 0.169208 1.010401 0.254875 41.00000 -1.50000
H14B 2 0.163020 1.073996 0.190097 41.00000 -1.50000
H14C 2 0.134482 0.982623 0.175175 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C14A 1 0.080280 1.027179 0.236252 -41.00000 0.03711 0.03702 =
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AFIX 137
H14D 2 0.105613 1.014997 0.285247 -41.00000 -1.50000
H14E 2 0.101519 1.080522 0.222038 -41.00000 -1.50000
H14F 2 0.103282 0.987342 0.202263 -41.00000 -1.50000
AFIX 0
PART 0
PART 1
C15 1 -0.040260 0.931144 0.352779 41.00000 0.03528 0.05292 =
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AFIX 13
H15 2 -0.067862 0.876366 0.357645 41.00000 -1.20000
AFIX 0
PART 0
PART 2
C15A 1 -0.057109 0.891237 0.360442 -41.00000 0.03383 0.04898 =
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AFIX 13
H15A 2 -0.068738 0.832285 0.362986 -41.00000 -1.20000
AFIX 0
PART 0
PART 1
C16 1 -0.097694 0.984511 0.404173 41.00000 0.04415 0.04687 =
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AFIX 137
H16A 2 -0.071888 1.038957 0.404462 41.00000 -1.50000
H16B 2 -0.092883 0.962469 0.453345 41.00000 -1.50000
H16C 2 -0.164503 0.985737 0.387097 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C16A 1 -0.128260 0.930841 0.410859 -41.00000 0.03900
AFIX 137
H16D 2 -0.129022 0.988768 0.402692 -41.00000 -1.50000
H16E 2 -0.108911 0.919823 0.461465 -41.00000 -1.50000
H16F 2 -0.191935 0.909028 0.400369 -41.00000 -1.50000
AFIX 0
PART 0
PART 1
C17 1 0.064741 0.922996 0.382049 41.00000 0.03834 0.04918 =
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AFIX 137
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H17B 2 0.066030 0.900259 0.430973 41.00000 -1.50000
H17C 2 0.094799 0.975873 0.383527 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C17A 1 0.045499 0.905142 0.391934 -41.00000 0.03871 0.05629 =
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AFIX 137
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H17E 2 0.053834 0.877540 0.438571 -41.00000 -1.50000
H17F 2 0.056330 0.962587 0.398928 -41.00000 -1.50000
AFIX 0
PART 0
PART 1
C18 1 -0.179354 0.984245 0.220780 41.00000 0.03043 0.05640 =
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AFIX 13
H18 2 -0.181639 0.984325 0.166584 41.00000 -1.20000
AFIX 0
PART 0
PART 2
C18A 1 -0.215738 0.924234 0.238822 -41.00000 0.02608 0.05888 =
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AFIX 13
H18A 2 -0.244290 0.954472 0.279238 -41.00000 -1.20000
AFIX 0
PART 0
PART 1
C19 1 -0.213164 1.069132 0.242339 41.00000 0.03991 0.06102 =
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AFIX 137
H19A 2 -0.215595 1.072583 0.295177 41.00000 -1.50000
H19B 2 -0.276569 1.079136 0.220303 41.00000 -1.50000
H19C 2 -0.168646 1.109202 0.225130 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C19A 1 -0.240933 0.971505 0.168155 -41.00000 0.03524 0.05923 =
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AFIX 137
H19D 2 -0.209046 1.023611 0.170104 -41.00000 -1.50000
H19E 2 -0.309832 0.979469 0.163433 -41.00000 -1.50000
H19F 2 -0.219809 0.941247 0.126365 -41.00000 -1.50000
AFIX 0
PART 0
PART 1
C20 1 -0.253517 0.920392 0.241828 41.00000 0.03708 0.06480 =
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AFIX 137
H20A 2 -0.317727 0.940849 0.230899 41.00000 -1.50000
H20B 2 -0.245790 0.908775 0.293739 41.00000 -1.50000
H20C 2 -0.243779 0.871306 0.214111 41.00000 -1.50000
AFIX 0
PART 0
PART 2
C20A 1 -0.262423 0.840085 0.237525 -41.00000 0.03410 0.06520 =
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AFIX 137
H20D 2 -0.238069 0.808793 0.197490 -41.00000 -1.50000
H20E 2 -0.331480 0.845668 0.230809 -41.00000 -1.50000
H20F 2 -0.247187 0.812680 0.283458 -41.00000 -1.50000
AFIX 0
PART 0
C21 1 -0.043721 0.774960 0.225777 11.00000 0.03583 0.12567 =
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AFIX 23
H21A 2 -0.086979 0.778561 0.266491 11.00000 -1.20000
H21B 2 -0.076998 0.745755 0.185547 11.00000 -1.20000
AFIX 0
C22 1 0.045176 0.730653 0.249682 11.00000 0.05404 0.07299 =
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AFIX 23
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H22B 2 0.079155 0.760076 0.289448 11.00000 -1.20000
AFIX 0
N3 3 0.217956 0.850318 0.124907 11.00000 0.03115 0.04563 =
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PART 1
SI3 4 0.325483 0.890654 0.090484 21.00000 0.03035 0.03002 =
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PART 0
PART 2
SI3A 4 0.323681 0.856410 0.069677 -21.00000 0.02882 0.03033 =
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PART 0
PART 1
C23 1 0.282112 0.925441 -0.005371 21.00000 0.03302 0.03650 =
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AFIX 13
H23 2 0.235643 0.969819 0.001247 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C23A 1 0.293081 0.868300 -0.033667 -21.00000 0.03412 0.03750 =
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AFIX 13
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AFIX 0
PART 0
PART 1
C24 1 0.229248 0.859087 -0.050401 21.00000 0.04582 0.04629 =
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AFIX 137
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H24B 2 0.199091 0.882759 -0.094136 21.00000 -1.50000
H24C 2 0.180567 0.834622 -0.021215 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C24A 1 0.222448 0.806468 -0.067792 -21.00000 0.04335 0.04152 =
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AFIX 137
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H24E 2 0.200533 0.824784 -0.116055 -21.00000 -1.50000
H24F 2 0.167896 0.800895 -0.037021 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C25 1 0.363306 0.959711 -0.050448 21.00000 0.04253 0.05532 =
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AFIX 137
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H25B 2 0.338717 0.971526 -0.099717 21.00000 -1.50000
H25C 2 0.414626 0.920300 -0.052388 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C25A 1 0.380850 0.870730 -0.082230 -21.00000 0.04389 0.05158 =
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AFIX 137
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H25E 2 0.359549 0.880503 -0.132651 -21.00000 -1.50000
H25F 2 0.414423 0.819432 -0.078866 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C26 1 0.421470 0.807447 0.092937 21.00000 0.03395 0.03329 =
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AFIX 13
H26 2 0.425909 0.787085 0.143888 21.00000 -1.20000
AFIX 0
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PART 2
C26A 1 0.411363 0.767762 0.087552 -21.00000 0.03445 0.03463 =
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AFIX 13
H26A 2 0.405939 0.752969 0.139678 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C27 1 0.398152 0.734247 0.044263 21.00000 0.04095 0.03468 =
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AFIX 137
H27A 2 0.343926 0.705361 0.063059 21.00000 -1.50000
H27B 2 0.453408 0.698649 0.044125 21.00000 -1.50000
H27C 2 0.382336 0.752313 -0.005259 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C27A 1 0.386637 0.690559 0.043160 -21.00000 0.04429 0.03557 =
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AFIX 137
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H27E 2 0.427153 0.646447 0.060857 -21.00000 -1.50000
H27F 2 0.397404 0.700123 -0.008170 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C28 1 0.522471 0.837120 0.075679 21.00000 0.03458 0.04011 =
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AFIX 137
H28A 2 0.517601 0.888122 0.049628 21.00000 -1.50000
H28B 2 0.553328 0.797424 0.045536 21.00000 -1.50000
H28C 2 0.560217 0.844537 0.120984 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C28A 1 0.518050 0.786022 0.077622 -21.00000 0.03681 0.03817 =
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AFIX 137
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H28E 2 0.554812 0.736401 0.082498 -21.00000 -1.50000
H28F 2 0.540687 0.824279 0.114671 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C29 1 0.384023 0.980741 0.139724 21.00000 0.03704 0.03306 =
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AFIX 13
H29 2 0.435186 0.999793 0.108012 21.00000 -1.20000
AFIX 0
PART 0
PART 2
C29A 1 0.397230 0.951889 0.093602 -21.00000 0.03456 0.03361 =
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AFIX 13
H29A 2 0.458660 0.948656 0.068553 -21.00000 -1.20000
AFIX 0
PART 0
PART 1
C30 1 0.432793 0.965538 0.215268 21.00000 0.05439 0.04181 =
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AFIX 137
H30A 2 0.386765 0.973841 0.252834 21.00000 -1.50000
H30B 2 0.486036 1.002737 0.222955 21.00000 -1.50000
H30C 2 0.456416 0.910424 0.217783 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C30A 1 0.419847 0.958261 0.176092 -21.00000 0.04696 0.04144 =
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AFIX 137
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H30E 2 0.465953 1.001297 0.185572 -21.00000 -1.50000
H30F 2 0.446539 0.907506 0.194035 -21.00000 -1.50000
AFIX 0
PART 0
PART 1
C31 1 0.311692 1.050490 0.143306 21.00000 0.03659 0.03639 =
0.07798 -0.00509 -0.00753 -0.00975
AFIX 137
H31A 2 0.256331 1.038968 0.111056 21.00000 -1.50000
H31B 2 0.341677 1.100249 0.128021 21.00000 -1.50000
H31C 2 0.291390 1.056301 0.193102 21.00000 -1.50000
AFIX 0
PART 0
PART 2
C31A 1 0.345083 1.029109 0.068242 -21.00000 0.04169 0.02921 =
0.06483 0.00318 -0.00314 -0.00414
AFIX 137
H31D 2 0.354458 1.037584 0.016554 -21.00000 -1.50000
H31E 2 0.370717 1.074849 0.095908 -21.00000 -1.50000
H31F 2 0.277058 1.023784 0.076209 -21.00000 -1.50000
AFIX 0
PART 0
C32 1 0.237774 0.821844 0.203213 11.00000 0.03911 0.04505 =
0.06206 0.00918 -0.00571 -0.00855
AFIX 23
H32A 2 0.198482 0.852431 0.236710 11.00000 -1.20000
H32B 2 0.305531 0.830202 0.217702 11.00000 -1.20000
AFIX 0
C33 1 0.212480 0.730419 0.206456 11.00000 0.04222 0.04262 =
0.05323 0.01572 -0.00596 0.00290
AFIX 23
H33A 2 0.250958 0.699699 0.172503 11.00000 -1.20000
H33B 2 0.225178 0.709352 0.256023 11.00000 -1.20000
AFIX 0
N4 3 0.107839 0.723524 0.185096 11.00000 0.04030 0.04471 =
0.03973 -0.00500 -0.00954 -0.01111
HKLF 4
REM UBMGNF in P21/n #14
REM R1 = 0.0814 for 7122 Fo > 4sig(Fo) and 0.0897 for all 8115 data
REM 680 parameters refined using 1911 restraints
END
WGHT 0.1131 60.9348
REM Highest difference peak 5.899, deepest hole -2.262, 1-sigma level 0.337
Q1 1 0.0535 0.8521 0.0483 11.00000 0.05 5.90
Q2 1 0.0809 0.8547 0.1437 11.00000 0.05 5.84
Q3 1 0.0572 0.8999 0.0961 11.00000 0.05 3.92
Q4 1 0.0585 0.8039 0.0989 11.00000 0.05 3.67
Q5 1 0.0070 0.9972 0.0511 11.00000 0.05 3.38
Q6 1 -0.0004 0.9566 0.0081 11.00000 0.05 1.98
Q7 1 -0.0176 0.8612 0.1100 11.00000 0.05 1.92
Q8 1 0.0789 0.9771 0.0997 11.00000 0.05 1.68
Q9 1 0.2056 0.8585 0.1427 11.00000 0.05 1.61
Q10 1 -0.0639 0.8778 0.0338 11.00000 0.05 1.60
Q11 1 0.1614 0.8547 0.0884 11.00000 0.05 1.54
Q12 1 -0.0104 0.8750 0.0052 11.00000 0.05 1.53
Q13 1 -0.0613 0.9781 0.2540 11.00000 0.05 1.43
Q14 1 0.0984 0.9054 -0.0166 11.00000 0.05 1.37
Q15 1 0.0528 0.7291 0.0934 11.00000 0.05 1.33
Q16 1 0.1204 0.9724 0.0713 11.00000 0.05 1.27
Q17 1 -0.0651 0.9037 0.2439 11.00000 0.05 1.23
Q18 1 0.3409 0.8565 0.0491 11.00000 0.05 1.19
Q19 1 -0.0236 0.7162 0.0006 11.00000 0.05 1.11
Q20 1 0.0430 0.7837 -0.0018 11.00000 0.05 1.09
;
_shelx_res_checksum 92642
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
7 1 -8 0.1017 7.0068 1.0363 -7.9796 -0.9954 0.2176 -0.0316
5 -9 -4 0.0859 5.0252 -8.9890 -4.0318 -0.7209 -0.7427 -0.2458
4 3 10 0.2009 3.9888 3.0106 10.0235 0.2999 0.3714 -0.9026
2 10 -4 0.0919 1.9815 10.0253 -3.9478 -0.2745 0.9603 0.2142
2 -8 -8 0.0716 2.0241 -7.9957 -8.0339 -0.7073 -0.7146 0.2505
-2 10 0 0.1153 -2.0232 10.0059 0.0433 0.2677 0.8881 0.2748
-7 5 5 0.1338 -7.0181 4.9747 5.0082 0.8895 0.3342 0.2911
-6 -3 8 0.1001 -6.0018 -3.0351 7.9723 0.8952 -0.3835 -0.0701
6 -3 8 0.1672 6.0045 -2.9880 7.9993 -0.0385 -0.1488 -1.0044
-8 -3 5 0.1185 -8.0009 -3.0402 4.9677 0.8776 -0.4271 0.2737
1 10 3 0.1329 0.9764 10.0149 3.0501 0.2076 0.9512 -0.1468
-2 -9 -5 0.0856 -1.9778 -9.0156 -5.0476 -0.2340 -0.8811 0.3619
-5 5 -7 0.1197 -5.0091 4.9937 -6.9875 0.0409 0.3553 0.8877
0 2 -12 0.1009 0.0035 2.0139 -11.9906 -0.6705 0.1675 0.7761
9 0 1 0.1113 9.0041 0.0344 1.0203 -0.6425 0.1775 -0.7634
1 7 -9 0.0932 0.9910 7.0219 -8.9644 -0.5190 0.6551 0.5697
_olex2_submission_special_instructions 'No special instructions were received'