University of Groningen The 6-amino-6-methyl-1,4-diazepine group as an ancillary ligand

62 Pages·2006·0.28 MB·English

University of Groningen

The 6-amino-6-methyl-1,4-diazepine group as an ancillary ligand framework for neutral and
cationic scandium and yttrium alkyls
Ge, Shaozhong; Bambirra, Sergio; Meetsma, Auke; Hessen, Bart
Published in:
Chemical Communications
DOI:
10.1039/b606384e
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Document Version
Publisher's PDF, also known as Version of record
Publication date:
2006
Link to publication in University of Groningen/UMCG research database
Citation for published version (APA):
Ge, S., Bambirra, S., Meetsma, A., & Hessen, B. (2006). The 6-amino-6-methyl-1,4-diazepine group as an
ancillary ligand framework for neutral and cationic scandium and yttrium alkyls. Chemical Communications,
233(31), 3320-3322. https://doi.org/10.1039/b606384e
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# Supplementary Material (ESI) for Chemical Communications
# This journal is (c) The Royal Society of Chemistry 2006
data_global
_journal_name_full Chem.Commun.
_journal_coden_Cambridge 0182
_publ_contact_author_address
;
Stratingh Institute
University of Groningen
Nijenborgh 4
Groningen
9747 AG
NETHERLANDS
;
_publ_contact_author_email [email protected]
_publ_contact_author_name 'Bart Hessen'
_publ_contact_letter # Include date of submission
;
Date of submission : 2006-05-01 11:34:17
Consider this CIF submission for deposition of the first
X-ray structure of a manuscript to be submitted to : Chem. Comm
(Our Compound_Identification_Code : Q1079)
;
_publ_section_title
;
The 6-amino-6-methyl-1,4-diazepine group as ancillary
ligand framework for neutral and cationic scandium and yttrium alkyls
;
loop_
_publ_author_name
'Bart Hessen'
'Sergio Bambirra'
'Shaozhong Ge'
'Auke Meetsma'
data_Q1079
_database_code_depnum_ccdc_archive 'CCDC 606108'
#==============================================================================
# 0. AUDIT DETAILS
_audit_creation_date '2006-01-31 16:44:17'
_audit_creation_method
;
PLATON <TABLE ACC> option (version :: 300106)
SHELXL97-2 & Manual Editing
;
_audit_update_record
;
?
;
# Insert blank lines between references
_publ_section_references
;
Allen, F.H. (2000). Acta Cryst. B58, 380-388.
Beurskens, P.T., Beurskens, G., Gelder, R. de, Garc\'ia-Granda, S.
Gould, R.O., Israel, & Smits, J.M.M. (1999).
The DIRDIF99 program system, Technical Report of the Crystallography
Laboratory, University of Nijmegen, The Netherlands.
Bondi, A. (1964). J. Phys. Chem. 68, 441-451.
Bruker, (2000). SMART, SAINTPLUS and XPREP.
Software Reference Manual Bruker AXS Inc. Madison, Wisconsin, USA.
Hahn, T. (1983) Ed. International Tables for Crystallography,
Volume A, Space-group symmetry, Kluwer Academic Publishers,
Dordrecht, The Netherlands.
Le Page, Y. (1987). J. Appl. Cryst. 20, 264-269.
Le Page, Y. (1988). J. Appl. Cryst. 21, 983-984.
Meetsma, A. (2005). Extended version of the program PLUTO.
Groningen University, The Netherlands. (unpublished).
Sheldrick, G.M. SHELXL97. Program for Crystal Structure
Refinement. University of Gottingen, Germany, 1997.
Sheldrick, G.M. SADABS. Version 2.03
Multi-Scan Absorption Correction Program.
University of Gottingen, Germany, 2001
Spek, A.L. (1987). Acta Cryst. C43, 1233-1235.
Spek, A.L. (1988). J. Appl. Cryst. 21, 578-579.
Spek, A.L. (1990). Acta Cryst. A46, C-34.
Spek, A.L. (2003). J. Appl. Cryst. 36, 7-13.
Wilson, A.J.C. (1992) Ed. International Tables for Crystallography,
Volume C, Kluwer Academic Publishers, Dordrecht, The Netherlands.
;
_publ_section_figure_captions
;
Fig. 1. Perspective PLUTO drawing of the moolecule illustrating the
configuration and the adopted numbering scheme.
Fig. 2. Molecular packing viewed down unit cell axes.
Fig. 3. Perspective ORTEP drawing of the title compound.
Displacement ellipsoids for non-H are represented at the 50%
probability level.
The H-atoms have been omitted to improve clarity.
;
#===============================================================================
# 5. CHEMICAL DATA
_chemical_name_systematic
;
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_formula_moiety 'C22 H56 N3 Sc Si3'
# Ex: 'C12 H16 N2 O6, H2 O' and '(Cd 2+)3, (C6 N6 Cr 3-)2, 2(H2 O)'
_chemical_formula_structural ?
_chemical_formula_sum 'C22 H56 N3 Sc Si3'
_chemical_formula_iupac ?
_chemical_formula_weight 491.92
_chemical_compound_source 'see text'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.2519 0.3716 '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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
#===============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting Monoclinic
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_space_group_name_H-M 'P 21/c'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,1/2+y,1/2-z
3 -x,-y,-z
4 x,1/2-y,1/2+z
_cell_length_a 18.418(1)
_cell_length_b 17.990(1)
_cell_length_c 18.694(1)
_cell_angle_alpha 90
_cell_angle_beta 95.799(1)
_cell_angle_gamma 90
_cell_volume 6162.4(6)
_cell_formula_units_Z 8
_cell_measurement_temperature 100(1)
_cell_measurement_reflns_used 7628
_cell_measurement_theta_min 2.19
_cell_measurement_theta_max 27.85
_cell_special_details
;
The final unit cell was obtained from the xyz centroids of
7628 reflections after integration using the SAINT software
package (Bruker, 2000).
;
_exptl_crystal_description block
_exptl_crystal_colour colorless
_exptl_crystal_size_max 0.28
_exptl_crystal_size_mid 0.21
_exptl_crystal_size_min 0.13
_exptl_crystal_size_rad ?
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.060
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 2176
_exptl_absorpt_coefficient_mu 0.368
_exptl_absorpt_correction_type Multi-Scan
_exptl_absorpt_process_details '(SADABS, Sheldrick, Bruker, 2001))'
_exptl_absorpt_correction_T_min 0.8804
_exptl_absorpt_correction_T_max 0.9534
#===============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 100(1)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'fine focus sealed Siemens Mo tube '
_diffrn_radiation_monochromator 'parallel mounted graphite'
_diffrn_radiation_detector
;
CCD area-detector
;
_diffrn_measurement_device_type
;
Bruker Smart Apex; CCD area detector
;
_diffrn_measurement_method '\f and \w scans'
_diffrn_special_details
;
Crystal into the cold nitrogen stream of the low-temparature unit
(KRYOFLEX, (Bruker, 2000)).
;
_diffrn_detector_area_resol_mean '4096x4096 / 62x62 (binned 512)'
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% 0
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
# number of measured reflections (redundant set)
_diffrn_reflns_number 41674
_diffrn_reflns_av_R_equivalents 0.1157
_diffrn_reflns_av_sigmaI/netI 0.1319
_diffrn_reflns_limit_h_min -22
_diffrn_reflns_limit_h_max 18
_diffrn_reflns_limit_k_min -22
_diffrn_reflns_limit_k_max 22
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_limit_l_max 23
_diffrn_reflns_theta_min 2.26
_diffrn_reflns_theta_max 26.02
_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_reduction_process
;
Intensity data were corrected for Lorentz and polarization
effects, decay and absorption and reduced to F~o~^2^
using SAINT (Bruker, 2000) and SADABS (Sheldrick, 2001)
;
# number of unique reflections
_reflns_number_total 12024
_reflns_number_gt 7135
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART, Version 5.624, (Bruker, 2001)'
_computing_cell_refinement 'SAINTPLUS, Version 6.02A, (Bruker, 2000)'
_computing_data_reduction 'XPREP, Version 5.1/NT, (Bruker, 2000)'
_computing_structure_solution
;
DIRDIF-99 (Beurskens et al., 1999)
;
_computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics
;
PLUTO (Meetsma, 2005)
PLATON (Spek, 2003)
;
_computing_publication_material 'PLATON (Spek, 2003)'
#===============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.0P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary heavy
_atom_sites_solution_secondary direct
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment refall
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_abs_structure_details ?
_chemical_absolute_configuration ?
_refine_ls_abs_structure_Flack ?
_refine_ls_number_reflns 12024
_refine_ls_number_parameters 971
_refine_ls_number_restraints 0
_refine_ls_number_constraints ?
_refine_ls_R_factor_all 0.1162
_refine_ls_R_factor_gt 0.0544
_refine_ls_wR_factor_ref 0.1084
_refine_ls_wR_factor_gt 0.0908
_refine_ls_goodness_of_fit_ref 0.964
_refine_ls_restrained_S_all 0.964
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_diff_density_max 0.393
_refine_diff_density_min -0.358
_refine_diff_density_rms 0.076
_vrn_publ_code_squeezed_elec 0.0
_vrn_publ_code_void_volume 0.0
_vrn_publ_code_frame_time_sec 10.0
_vrn_publ_code_meas_time_hour 7.0
#===============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_U_iso_or_equiv
_atom_site_calc_flag
_atom_site_refinement_flags
Sc1 Sc Uani 0.56844(3) 0.12363(3) 0.31174(3) 1.000 0.0121(2) . .
Si11 Si Uani 0.68628(5) 0.29695(5) 0.29317(5) 1.000 0.0166(3) . .
Si12 Si Uani 0.70520(5) 0.08852(5) 0.46532(5) 1.000 0.0173(3) . .
Si13 Si Uani 0.44720(5) 0.22201(5) 0.43613(5) 1.000 0.0173(3) . .
N11 N Uani 0.61089(14) 0.07532(13) 0.19743(13) 1.000 0.0151(9) . .
N12 N Uani 0.50884(15) 0.00192(14) 0.28995(13) 1.000 0.0165(9) . .
N13 N Uani 0.46533(14) 0.12556(14) 0.21224(14) 1.000 0.0152(9) . .
C11 C Uani 0.6809(2) 0.0334(2) 0.2027(2) 1.000 0.0203(12) . .
C12 C Uani 0.6237(2) 0.14139(19) 0.15199(19) 1.000 0.0177(11) . .
C13 C Uani 0.54763(18) 0.02821(17) 0.16595(16) 1.000 0.0152(11) . .
C14 C Uani 0.5335(2) -0.03038(18) 0.22274(19) 1.000 0.0194(11) . .
C15 C Uani 0.5250(3) -0.0526(2) 0.3496(2) 1.000 0.0239(14) . .
C16 C Uani 0.4283(2) 0.0142(2) 0.2795(2) 1.000 0.0237(12) . .
C17 C Uani 0.4072(2) 0.0905(2) 0.2492(2) 1.000 0.0214(12) . .
C18 C Uani 0.4377(2) 0.1995(2) 0.1856(2) 1.000 0.0235(12) . .
C19 C Uani 0.4811(2) 0.0785(2) 0.15028(19) 1.000 0.0182(12) . .
C110 C Uani 0.5612(2) -0.0120(2) 0.0968(2) 1.000 0.0231(14) . .
C111 C Uani 0.6020(2) 0.24420(18) 0.3022(2) 1.000 0.0183(11) . .
C112 C Uani 0.6850(3) 0.3365(2) 0.1999(2) 1.000 0.0269(14) . .
C113 C Uani 0.7735(2) 0.2416(2) 0.3078(2) 1.000 0.0257(12) . .
C114 C Uani 0.6976(3) 0.3764(2) 0.3594(2) 1.000 0.0268(14) . .
C115 C Uani 0.6706(2) 0.0750(2) 0.37035(18) 1.000 0.0167(12) . .
C116 C Uani 0.8056(2) 0.0664(2) 0.4832(2) 1.000 0.0272(14) . .
C117 C Uani 0.6942(2) 0.1870(2) 0.4956(2) 1.000 0.0210(14) . .
C118 C Uani 0.6559(3) 0.0265(2) 0.5256(2) 1.000 0.0310(14) . .
C119 C Uani 0.4950(2) 0.14065(19) 0.40346(18) 1.000 0.0182(12) . .
C120 C Uani 0.5120(2) 0.2918(2) 0.4821(2) 1.000 0.0249(14) . .
C121 C Uani 0.3821(2) 0.1980(2) 0.5037(2) 1.000 0.0272(14) . .
C122 C Uani 0.3920(2) 0.2759(2) 0.3641(2) 1.000 0.0243(14) . .
H11 H Uiso 0.6958(16) 0.0217(15) 0.1522(16) 1.000 0.014(8) . .
H11' H Uiso 0.6767(17) -0.0108(18) 0.2292(16) 1.000 0.023(10) . .
H11" H Uiso 0.7191(17) 0.0656(16) 0.2291(16) 1.000 0.018(9) . .
H12 H Uiso 0.6694(16) 0.1646(15) 0.1741(14) 1.000 0.008(8) . .
H12' H Uiso 0.5837(18) 0.1806(18) 0.1532(16) 1.000 0.029(10) . .
H12" H Uiso 0.6289(16) 0.1282(16) 0.1004(17) 1.000 0.021(9) . .
H14 H Uiso 0.4957(17) -0.0647(16) 0.2017(15) 1.000 0.016(8) . .
H14' H Uiso 0.5823(16) -0.0586(15) 0.2399(15) 1.000 0.012(8) . .
H15 H Uiso 0.4974(17) -0.1026(17) 0.3393(16) 1.000 0.023(9) . .
H15' H Uiso 0.5074(16) -0.0324(15) 0.3918(16) 1.000 0.009(8) . .
H15" H Uiso 0.580(2) -0.0607(18) 0.3530(18) 1.000 0.035(11) . .
H16 H Uiso 0.4100(16) 0.0080(15) 0.3243(16) 1.000 0.009(9) . .
H16' H Uiso 0.4069(16) -0.0236(16) 0.2499(16) 1.000 0.017(9) . .
H17 H Uiso 0.3631(16) 0.0904(14) 0.2168(15) 1.000 0.009(8) . .
H17' H Uiso 0.3975(15) 0.1228(15) 0.2890(16) 1.000 0.008(8) . .
H18 H Uiso 0.3931(18) 0.1935(16) 0.1552(17) 1.000 0.022(9) . .
H18' H Uiso 0.4739(19) 0.2218(17) 0.1578(17) 1.000 0.025(10) . .
H18" H Uiso 0.4291(16) 0.2298(16) 0.2272(17) 1.000 0.016(9) . .
H19 H Uiso 0.4906(16) 0.1106(16) 0.1131(16) 1.000 0.012(9) . .
H19' H Uiso 0.4378(16) 0.0477(15) 0.1336(15) 1.000 0.013(8) . .
H110 H Uiso 0.5738(18) 0.0212(18) 0.0595(18) 1.000 0.029(10) . .
H110' H Uiso 0.518(2) -0.0335(18) 0.0776(18) 1.000 0.034(11) . .
H110" H Uiso 0.5978(18) -0.0528(18) 0.1049(16) 1.000 0.028(10) . .
H111 H Uiso 0.566(2) 0.268(2) 0.271(2) 1.000 0.048(12) . .
H111' H Uiso 0.5906(19) 0.2522(18) 0.3468(19) 1.000 0.032(11) . .
H112 H Uiso 0.6896(19) 0.299(2) 0.1680(19) 1.000 0.038(12) . .
H112' H Uiso 0.723(2) 0.370(2) 0.196(2) 1.000 0.058(14) . .
H112" H Uiso 0.644(2) 0.364(2) 0.186(2) 1.000 0.051(13) . .
H113 H Uiso 0.784(2) 0.218(2) 0.356(2) 1.000 0.047(12) . .
H113' H Uiso 0.815(2) 0.272(2) 0.3012(18) 1.000 0.039(12) . .
H113" H Uiso 0.7733(18) 0.2084(18) 0.2723(18) 1.000 0.023(10) . .
H114 H Uiso 0.656(2) 0.408(2) 0.3580(19) 1.000 0.042(12) . .
H114' H Uiso 0.740(2) 0.405(2) 0.355(2) 1.000 0.049(13) . .
H114" H Uiso 0.7055(17) 0.3570(17) 0.4070(18) 1.000 0.025(10) . .
H115 H Uiso 0.6746(17) 0.0227(18) 0.3604(16) 1.000 0.025(9) . .
H115' H Uiso 0.7029(19) 0.0960(18) 0.3465(18) 1.000 0.027(11) . .
H116 H Uiso 0.816(2) 0.017(2) 0.4734(18) 1.000 0.045(12) . .
H116' H Uiso 0.8219(19) 0.0749(18) 0.531(2) 1.000 0.037(11) . .
H116" H Uiso 0.833(2) 0.097(2) 0.456(2) 1.000 0.063(16) . .
H117 H Uiso 0.7125(19) 0.2215(19) 0.4648(19) 1.000 0.036(11) . .
H117' H Uiso 0.7192(18) 0.1935(17) 0.5448(19) 1.000 0.032(10) . .
H117" H Uiso 0.642(2) 0.1962(18) 0.4970(18) 1.000 0.036(11) . .
H118 H Uiso 0.603(2) 0.036(2) 0.521(2) 1.000 0.056(14) . .
H118' H Uiso 0.672(2) 0.0355(19) 0.578(2) 1.000 0.050(12) . .
H118" H Uiso 0.666(2) -0.024(2) 0.5203(18) 1.000 0.043(12) . .
H119 H Uiso 0.4608(18) 0.1009(17) 0.4045(16) 1.000 0.027(10) . .
H119' H Uiso 0.5315(18) 0.1290(16) 0.4395(17) 1.000 0.019(9) . .
H120 H Uiso 0.5370(16) 0.2717(16) 0.5280(17) 1.000 0.018(9) . .
H120' H Uiso 0.485(2) 0.335(2) 0.4939(19) 1.000 0.045(12) . .
H120" H Uiso 0.549(2) 0.3091(18) 0.4549(18) 1.000 0.032(11) . .
H121 H Uiso 0.3439(19) 0.1682(18) 0.4859(17) 1.000 0.026(10) . .
H121' H Uiso 0.3585(19) 0.2375(19) 0.5215(18) 1.000 0.032(11) . .
H121" H Uiso 0.4083(19) 0.1731(18) 0.5410(19) 1.000 0.033(11) . .
H122 H Uiso 0.4209(19) 0.3017(18) 0.3331(18) 1.000 0.027(10) . .
H122' H Uiso 0.3633(17) 0.3089(17) 0.3836(16) 1.000 0.016(9) . .
H122" H Uiso 0.3570(18) 0.2425(18) 0.3348(17) 1.000 0.028(10) . .
Sc2 Sc Uani 0.09137(3) 0.14360(3) 0.20218(3) 1.000 0.0128(2) . .
Si21 Si Uani -0.08889(5) 0.20152(5) 0.09287(5) 1.000 0.0204(3) . .
Si22 Si Uani 0.16272(5) 0.33840(5) 0.18764(5) 1.000 0.0208(3) . .
Si23 Si Uani 0.18384(6) 0.10156(5) 0.03536(5) 1.000 0.0237(3) . .
N21 N Uani 0.01502(15) 0.13335(14) 0.30466(14) 1.000 0.0174(9) . .
N22 N Uani 0.17295(15) 0.09715(14) 0.30485(14) 1.000 0.0167(9) . .
N23 N Uani 0.07188(14) 0.00865(14) 0.23165(14) 1.000 0.0164(9) . .
C21 C Uani 0.0075(3) 0.2019(2) 0.3478(2) 1.000 0.0303(14) . .
C22 C Uani -0.0604(2) 0.1146(2) 0.2745(2) 1.000 0.0237(12) . .
C23 C Uani 0.05044(18) 0.07037(18) 0.34878(17) 1.000 0.0182(11) . .
C24 C Uani 0.13079(19) 0.0917(2) 0.36854(19) 1.000 0.0222(12) . .
C25 C Uani 0.2376(2) 0.1454(2) 0.3235(2) 1.000 0.0253(12) . .
C26 C Uani 0.2006(2) 0.0219(2) 0.2868(2) 1.000 0.0243(12) . .
C27 C Uani 0.1472(2) -0.0213(2) 0.2345(2) 1.000 0.0237(14) . .
C28 C Uani 0.0262(3) -0.0349(2) 0.1765(2) 1.000 0.0265(14) . .
C29 C Uani 0.0442(2) -0.00031(19) 0.30307(18) 1.000 0.0197(11) . .
C210 C Uani 0.0171(2) 0.0552(2) 0.4193(2) 1.000 0.0273(16) . .
C211 C Uani -0.0021(2) 0.1524(2) 0.11478(19) 1.000 0.0215(12) . .
C212 C Uani -0.1715(2) 0.1457(3) 0.1099(3) 1.000 0.0274(16) . .
C213 C Uani -0.0937(3) 0.2912(2) 0.1442(3) 1.000 0.0349(16) . .
C214 C Uani -0.1015(3) 0.2280(4) -0.0046(3) 1.000 0.054(2) . .
C215 C Uani 0.1137(2) 0.26498(19) 0.2315(2) 1.000 0.0229(12) . .
C216 C Uani 0.1656(3) 0.4280(2) 0.2401(3) 1.000 0.0395(18) . .
C217 C Uani 0.1141(3) 0.3585(3) 0.0969(3) 1.000 0.0444(19) . .
C218 C Uani 0.2611(2) 0.3186(3) 0.1774(3) 1.000 0.0363(17) . .
C219 C Uani 0.1848(2) 0.1204(2) 0.1323(2) 1.000 0.0204(12) . .
C220 C Uani 0.1579(3) 0.1864(3) -0.0206(3) 1.000 0.050(2) . .
C221 C Uani 0.2752(3) 0.0719(3) 0.0092(3) 1.000 0.0385(17) . .
C222 C Uani 0.1194(3) 0.0252(3) 0.0040(3) 1.000 0.044(2) . .
H21 H Uiso -0.0071(19) 0.2417(19) 0.3167(18) 1.000 0.035(11) . .
H21' H Uiso 0.0576(18) 0.2133(16) 0.3727(16) 1.000 0.017(9) . .
H21" H Uiso -0.026(2) 0.1936(18) 0.3844(19) 1.000 0.036(12) . .
H22 H Uiso -0.088(2) 0.0994(18) 0.3142(19) 1.000 0.038(11) . .
H22' H Uiso -0.0600(15) 0.0727(16) 0.2370(16) 1.000 0.012(8) . .
H22" H Uiso -0.0843(18) 0.1591(19) 0.2561(17) 1.000 0.033(10) . .
H24 H Uiso 0.1349(16) 0.1420(17) 0.3909(16) 1.000 0.019(9) . .
H24' H Uiso 0.1523(17) 0.0575(16) 0.4036(16) 1.000 0.020(9) . .
H25 H Uiso 0.2234(16) 0.1913(16) 0.3387(15) 1.000 0.008(8) . .
H25' H Uiso 0.2633(18) 0.1540(17) 0.2795(18) 1.000 0.024(10) . .
H25" H Uiso 0.2742(18) 0.1204(16) 0.3620(17) 1.000 0.026(9) . .
H26 H Uiso 0.2121(16) -0.0060(16) 0.3313(16) 1.000 0.014(8) . .
H26' H Uiso 0.2449(19) 0.0302(18) 0.2648(17) 1.000 0.029(11) . .
H27 H Uiso 0.1610(17) -0.0174(16) 0.1838(17) 1.000 0.018(9) . .
H27' H Uiso 0.1471(19) -0.073(2) 0.2467(18) 1.000 0.044(11) . .
H28 H Uiso 0.0254(18) -0.086(2) 0.1934(18) 1.000 0.037(11) . .
H28' H Uiso 0.0498(17) -0.0296(16) 0.1283(18) 1.000 0.022(9) . .
H28" H Uiso -0.0230(19) -0.0168(17) 0.1718(17) 1.000 0.025(10) . .
H29 H Uiso 0.0715(16) -0.0407(16) 0.3305(15) 1.000 0.014(8) . .
H29' H Uiso -0.0094(16) -0.0161(14) 0.2944(14) 1.000 0.008(8) . .
H210 H Uiso 0.0244(18) 0.0980(18) 0.4539(18) 1.000 0.032(10) . .
H210' H Uiso 0.038(2) 0.009(2) 0.4417(19) 1.000 0.052(12) . .
H210" H Uiso -0.0344(19) 0.0480(16) 0.4101(16) 1.000 0.022(10) . .
H211 H Uiso 0.031(2) 0.175(2) 0.086(2) 1.000 0.051(13) . .
H211' H Uiso -0.0084(19) 0.104(2) 0.0952(18) 1.000 0.040(11) . .
H212 H Uiso -0.176(2) 0.104(2) 0.087(2) 1.000 0.070(16) . .
H212' H Uiso -0.216(2) 0.169(2) 0.093(2) 1.000 0.052(13) . .
H212" H Uiso -0.172(2) 0.132(2) 0.158(2) 1.000 0.061(14) . .
H213 H Uiso -0.089(2) 0.288(2) 0.198(2) 1.000 0.059(14) . .
H213' H Uiso -0.135(2) 0.3155(19) 0.1325(19) 1.000 0.036(12) . .
H213" H Uiso -0.050(2) 0.324(2) 0.1325(19) 1.000 0.048(12) . .
H214 H Uiso -0.063(3) 0.260(2) -0.013(2) 1.000 0.075(19) . .
H214' H Uiso -0.143(2) 0.255(2) -0.015(2) 1.000 0.064(15) . .
H214" H Uiso -0.097(2) 0.182(2) -0.036(2) 1.000 0.054(14) . .
H215 H Uiso 0.067(2) 0.2790(19) 0.2259(19) 1.000 0.042(12) . .
H215' H Uiso 0.1294(19) 0.2672(18) 0.2813(19) 1.000 0.037(11) . .
H216 H Uiso 0.121(2) 0.442(2) 0.253(2) 1.000 0.060(15) . .
H216' H Uiso 0.184(2) 0.471(2) 0.211(2) 1.000 0.071(15) . .
H216" H Uiso 0.198(2) 0.418(2) 0.290(2) 1.000 0.071(15) . .
H217 H Uiso 0.114(2) 0.316(2) 0.066(2) 1.000 0.054(14) . .
H217' H Uiso 0.145(2) 0.398(2) 0.076(2) 1.000 0.065(14) . .
H217" H Uiso 0.060(3) 0.381(3) 0.096(3) 1.000 0.098(19) . .
H218 H Uiso 0.286(2) 0.308(2) 0.222(2) 1.000 0.051(14) . .
H218' H Uiso 0.284(2) 0.361(2) 0.159(2) 1.000 0.050(12) . .
H218" H Uiso 0.269(2) 0.276(2) 0.149(2) 1.000 0.054(14) . .
H219 H Uiso 0.2051(19) 0.1604(19) 0.1411(18) 1.000 0.031(11) . .
H219' H Uiso 0.217(2) 0.086(2) 0.1552(19) 1.000 0.044(12) . .
H220 H Uiso 0.107(2) 0.2014(18) -0.0146(17) 1.000 0.029(10) . .
H220' H Uiso 0.154(3) 0.174(2) -0.069(3) 1.000 0.077(18) . .
H220" H Uiso 0.196(3) 0.225(3) -0.011(2) 1.000 0.085(19) . .
H221 H Uiso 0.311(2) 0.110(2) 0.023(2) 1.000 0.049(13) . .
H221' H Uiso 0.280(2) 0.066(2) -0.036(2) 1.000 0.055(15) . .
H221" H Uiso 0.289(2) 0.026(2) 0.033(2) 1.000 0.061(14) . .
H222 H Uiso 0.125(2) -0.020(3) 0.031(2) 1.000 0.077(18) . .
H222' H Uiso 0.119(2) 0.0181(19) -0.047(2) 1.000 0.046(12) . .
H222" H Uiso 0.073(2) 0.039(2) 0.006(2) 1.000 0.060(16) . .
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
Sc1 0.0119(4) 0.0139(3) 0.0104(3) -0.0004(3) 0.0005(3) -0.0007(3)
Si11 0.0170(6) 0.0162(5) 0.0167(5) 0.0007(4) 0.0030(4) -0.0017(4)
Si12 0.0187(6) 0.0177(5) 0.0147(5) 0.0016(4) -0.0025(4) -0.0003(4)
Si13 0.0189(6) 0.0191(5) 0.0143(5) -0.0031(4) 0.0038(4) -0.0015(4)
N11 0.0122(17) 0.0177(15) 0.0149(15) 0.0017(12) -0.0016(13) 0.0030(12)
N12 0.0189(18) 0.0193(15) 0.0120(15) -0.0010(12) 0.0047(13) -0.0027(13)
N13 0.0124(17) 0.0178(14) 0.0153(15) 0.0011(12) 0.0014(13) 0.0033(12)
C11 0.017(2) 0.026(2) 0.018(2) -0.0015(18) 0.0019(18) 0.0061(17)
C12 0.019(2) 0.0190(19) 0.015(2) 0.0012(16) 0.0016(17) -0.0005(17)
C13 0.014(2) 0.0206(18) 0.0107(18) -0.0043(14) -0.0008(15) 0.0008(15)
C14 0.017(2) 0.0202(19) 0.021(2) -0.0045(16) 0.0014(17) -0.0048(16)
C15 0.034(3) 0.0158(19) 0.023(2) 0.0044(17) 0.009(2) -0.0043(18)
C16 0.017(2) 0.030(2) 0.024(2) -0.0040(18) 0.0020(19) -0.0079(17)
C17 0.010(2) 0.031(2) 0.022(2) -0.0053(18) -0.0047(17) -0.0002(16)
C18 0.020(2) 0.028(2) 0.023(2) 0.0008(19) 0.004(2) 0.0102(19)
C19 0.014(2) 0.025(2) 0.015(2) -0.0004(16) -0.0011(16) -0.0025(16)
C110 0.024(3) 0.029(2) 0.016(2) -0.0085(18) 0.0009(19) -0.0009(19)
C111 0.020(2) 0.0197(19) 0.016(2) -0.0007(16) 0.0058(18) 0.0019(16)
C112 0.032(3) 0.023(2) 0.026(2) 0.0002(19) 0.004(2) -0.001(2)
C113 0.021(2) 0.035(2) 0.021(2) -0.001(2) 0.0018(19) -0.0007(19)
C114 0.030(3) 0.025(2) 0.026(2) -0.0054(18) 0.006(2) -0.011(2)
C115 0.016(2) 0.019(2) 0.015(2) 0.0013(15) 0.0006(17) -0.0014(16)
C116 0.024(3) 0.030(2) 0.025(2) -0.006(2) -0.010(2) 0.0070(19)
C117 0.024(3) 0.023(2) 0.016(2) -0.0010(17) 0.0024(19) -0.0016(18)
C118 0.040(3) 0.028(2) 0.024(2) 0.0068(18) -0.002(2) -0.007(2)
C119 0.015(2) 0.023(2) 0.016(2) -0.0024(16) -0.0006(17) -0.0035(16)
C120 0.027(3) 0.027(2) 0.021(2) -0.0093(18) 0.004(2) -0.0020(19)
C121 0.027(3) 0.027(2) 0.028(2) -0.0010(19) 0.005(2) 0.004(2)
C122 0.032(3) 0.016(2) 0.026(2) -0.0047(18) 0.008(2) -0.0007(19)
Sc2 0.0114(4) 0.0136(3) 0.0133(3) 0.0006(3) 0.0015(3) 0.0016(3)
Si21 0.0130(6) 0.0269(5) 0.0211(6) 0.0071(4) 0.0008(4) 0.0031(4)
Si22 0.0163(6) 0.0148(5) 0.0307(6) 0.0025(4) 0.0002(5) -0.0002(4)
Si23 0.0218(6) 0.0302(6) 0.0200(6) 0.0000(4) 0.0069(5) 0.0042(5)
N21 0.0167(17) 0.0197(15) 0.0159(16) -0.0012(12) 0.0023(13) 0.0021(12)
N22 0.0157(17) 0.0205(15) 0.0135(15) 0.0000(12) -0.0005(13) 0.0005(12)
N23 0.0113(16) 0.0196(15) 0.0187(16) -0.0005(12) 0.0036(13) -0.0002(12)
C21 0.038(3) 0.032(2) 0.022(2) -0.0032(19) 0.009(2) 0.007(2)
C22 0.018(2) 0.030(2) 0.024(2) 0.0058(19) 0.0069(19) 0.0032(18)
C23 0.020(2) 0.0255(19) 0.0090(18) 0.0042(14) 0.0006(16) 0.0016(16)
C24 0.018(2) 0.034(2) 0.014(2) 0.0032(18) -0.0010(17) 0.0016(18)
C25 0.016(2) 0.037(2) 0.022(2) -0.001(2) -0.0027(19) -0.0031(19)
C26 0.017(2) 0.031(2) 0.025(2) 0.0087(18) 0.0027(19) 0.0089(18)
C27 0.021(2) 0.016(2) 0.035(3) 0.0039(17) 0.008(2) 0.0032(16)
C28 0.034(3) 0.019(2) 0.027(2) -0.0017(17) 0.005(2) -0.0066(19)
C29 0.018(2) 0.0218(19) 0.019(2) 0.0063(16) 0.0002(17) 0.0030(16)
C210 0.023(3) 0.040(3) 0.019(2) 0.0051(19) 0.0024(19) 0.002(2)
C211 0.018(2) 0.026(2) 0.020(2) 0.0000(17) -0.0002(18) 0.0027(17)
C212 0.020(3) 0.035(2) 0.028(3) 0.000(2) 0.006(2) -0.002(2)
C213 0.018(3) 0.027(2) 0.059(3) 0.004(2) 0.001(2) 0.006(2)
C214 0.038(4) 0.088(4) 0.036(3) 0.025(3) 0.003(3) 0.026(3)
C215 0.017(2) 0.025(2) 0.027(2) 0.0000(17) 0.0034(19) 0.0042(17)
C216 0.017(3) 0.021(2) 0.080(4) -0.007(2) 0.003(3) -0.0006(19)
C217 0.052(4) 0.035(3) 0.043(3) 0.016(2) -0.011(3) -0.018(3)
C218 0.025(3) 0.029(3) 0.056(3) 0.006(2) 0.010(2) -0.004(2)
C219 0.019(2) 0.020(2) 0.023(2) 0.0000(17) 0.0063(17) -0.0002(17)
C220 0.041(4) 0.068(4) 0.042(3) 0.024(3) 0.010(3) 0.016(3)
C221 0.040(3) 0.048(3) 0.031(3) 0.000(2) 0.021(2) 0.011(2)
C222 0.041(4) 0.060(4) 0.031(3) -0.023(3) 0.003(3) -0.003(3)
#===============================================================================
# 10. MOLECULAR GEOMETRY
_geom_special_details
;