# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2011
data_global
_journal_name_full 'Dalton Trans.'
_journal_coden_Cambridge 0222
_journal_volume ?
_journal_page_first ?
_journal_year ?
_publ_contact_author_name 'Dr Martyn Coles'
_publ_contact_author_email m.f.lappert@sussex.ac.uk
_publ_section_title
;
Crystalline metal (Li, Mg, Ca, Sr, Ba, Sn, Pb)
complexes of the new chelating N,N'-dianionic
[1,2-N(R)C6H4(CH2NR)]2-
ligand (R = SiMe3, CH2But)
;
_publ_requested_category FM
loop_
_publ_author_name
C.Caro
M.Coles
P.Hitchcock
M.Lappert
L.Pierssens
# Attachment '- Combined_cif.cif'
data_(4a)-nov1097
_database_code_depnum_ccdc_archive 'CCDC 819594'
#TrackingRef '- Combined_cif.cif'
_audit_creation_date 2011-03-17T10:19:30-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.2
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C26 H48 Li4 N4 Si4'
_chemical_formula_sum 'C26 H48 Li4 N4 Si4'
_chemical_formula_weight 556.8
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/n
_symmetry_space_group_name_Hall '-P 2yn'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z+1/2'
'-x, -y, -z'
'-x-1/2, y-1/2, -z-1/2'
_cell_length_a 9.729(2)
_cell_length_b 21.316(5)
_cell_length_c 16.744(4)
_cell_angle_alpha 90
_cell_angle_beta 97.90(2)
_cell_angle_gamma 90
_cell_volume 3439.5(14)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 7
_cell_measurement_theta_max 10
_cell_measurement_wavelength 0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description Block
_exptl_crystal_colour Colourless
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.3
_exptl_crystal_density_diffrn 1.075
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1200
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 0.193
_exptl_absorpt_correction_type none
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_measurement_device 'Enraf-Nonius CAD4'
_diffrn_measurement_method 'omega-2theta scans'
_diffrn_standards_number ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_av_R_equivalents 0.0602
_diffrn_reflns_av_unetI/netI 0.0783
_diffrn_reflns_number 6393
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 25
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_theta_min 2.27
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_full 24.98
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_reflns_number_total 6025
_reflns_number_gt 4032
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'Enraf-Nonius CAD4 software'
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_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^)+(0.0714P)^2^+1.2263P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 6025
_refine_ls_number_parameters 343
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0978
_refine_ls_R_factor_gt 0.0562
_refine_ls_wR_factor_ref 0.1511
_refine_ls_wR_factor_gt 0.1306
_refine_ls_goodness_of_fit_ref 0.998
_refine_ls_restrained_S_all 0.998
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.303
_refine_diff_density_min -0.324
_refine_diff_density_rms 0.061
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Li1 Li 0.3410(5) 0.8948(3) 0.3064(3) 0.0294(12) Uani 1 1 d . . .
Li2 Li 0.5199(6) 0.8159(3) 0.3183(3) 0.0321(13) Uani 1 1 d . . .
Li3 Li 0.3734(5) 0.9029(2) 0.1691(3) 0.0288(12) Uani 1 1 d . . .
Li4 Li 0.2079(6) 0.8179(3) 0.1469(3) 0.0340(13) Uani 1 1 d . . .
Si1 Si 0.36600(10) 0.80860(5) 0.46415(6) 0.0322(3) Uani 1 1 d . . .
Si2 Si 0.11029(9) 0.96340(4) 0.17217(6) 0.0268(2) Uani 1 1 d . . .
Si3 Si 0.37697(9) 0.83485(4) -0.00129(5) 0.0292(2) Uani 1 1 d . . .
Si4 Si 0.60181(9) 0.96625(4) 0.31377(6) 0.0296(2) Uani 1 1 d . . .
N1 N 0.3448(3) 0.80991(12) 0.36158(15) 0.0252(6) Uani 1 1 d . . .
N2 N 0.1846(3) 0.89615(12) 0.21399(15) 0.0242(6) Uani 1 1 d . . .
N3 N 0.3793(3) 0.82517(12) 0.10018(15) 0.0247(6) Uani 1 1 d . . .
N4 N 0.5310(3) 0.90107(12) 0.26386(15) 0.0249(6) Uani 1 1 d . . .
C1 C 0.2498(3) 0.76970(15) 0.31620(18) 0.0248(7) Uani 1 1 d . . .
C2 C 0.2718(4) 0.70485(16) 0.3125(2) 0.0357(8) Uani 1 1 d . . .
H2 H 0.353 0.6876 0.3425 0.043 Uiso 1 1 calc R . .
C3 C 0.1805(5) 0.66510(18) 0.2671(2) 0.0476(10) Uani 1 1 d . . .
H3 H 0.1992 0.6214 0.2667 0.057 Uiso 1 1 calc R . .
C4 C 0.0628(4) 0.68843(19) 0.2223(2) 0.0481(11) Uani 1 1 d . . .
H4 H -0.0009 0.6611 0.1914 0.058 Uiso 1 1 calc R . .
C5 C 0.0386(4) 0.75200(18) 0.2229(2) 0.0384(9) Uani 1 1 d . . .
H5 H -0.0412 0.7683 0.1905 0.046 Uiso 1 1 calc R . .
C6 C 0.1275(3) 0.79318(15) 0.26938(18) 0.0263(7) Uani 1 1 d . . .
C7 C 0.0973(3) 0.86242(15) 0.26670(19) 0.0290(8) Uani 1 1 d . . .
H7A H -0.0019 0.8692 0.2461 0.035 Uiso 1 1 calc R . .
H7B H 0.1153 0.8798 0.322 0.035 Uiso 1 1 calc R . .
C8 C 0.2552(4) 0.8679(2) 0.5071(2) 0.0504(11) Uani 1 1 d . . .
H8A H 0.2715 0.9094 0.4849 0.076 Uiso 1 1 calc R . .
H8B H 0.2788 0.8689 0.5659 0.076 Uiso 1 1 calc R . .
H8C H 0.1573 0.8566 0.493 0.076 Uiso 1 1 calc R . .
C9 C 0.5518(4) 0.8296(2) 0.4988(2) 0.0472(10) Uani 1 1 d . . .
H9A H 0.6127 0.7993 0.4771 0.071 Uiso 1 1 calc R . .
H9B H 0.5692 0.8288 0.5579 0.071 Uiso 1 1 calc R . .
H9C H 0.5706 0.8718 0.4796 0.071 Uiso 1 1 calc R . .
C10 C 0.3271(4) 0.73149(19) 0.5093(2) 0.0474(10) Uani 1 1 d . . .
H10A H 0.3831 0.6986 0.4887 0.071 Uiso 1 1 calc R . .
H10B H 0.2284 0.7217 0.4949 0.071 Uiso 1 1 calc R . .
H10C H 0.3495 0.7338 0.5681 0.071 Uiso 1 1 calc R . .
C11 C 0.0600(4) 1.02041(17) 0.2473(2) 0.0418(9) Uani 1 1 d . . .
H11A H -0.0103 1.0015 0.2764 0.063 Uiso 1 1 calc R . .
H11B H 0.022 1.0583 0.2194 0.063 Uiso 1 1 calc R . .
H11C H 0.1419 1.0315 0.2855 0.063 Uiso 1 1 calc R . .
C12 C -0.0497(4) 0.94938(17) 0.0987(2) 0.0392(9) Uani 1 1 d . . .
H12A H -0.0289 0.9195 0.0575 0.059 Uiso 1 1 calc R . .
H12B H -0.0812 0.9891 0.0729 0.059 Uiso 1 1 calc R . .
H12C H -0.1228 0.9322 0.1271 0.059 Uiso 1 1 calc R . .
C13 C 0.2440(4) 1.00159(16) 0.1181(2) 0.0366(8) Uani 1 1 d . . .
H13A H 0.2721 0.9724 0.078 0.055 Uiso 1 1 calc R . .
H13B H 0.325 1.0127 0.1569 0.055 Uiso 1 1 calc R . .
H13C H 0.2049 1.0396 0.0909 0.055 Uiso 1 1 calc R . .
C14 C 0.4774(3) 0.78358(14) 0.14174(18) 0.0257(7) Uani 1 1 d . . .
C15 C 0.4595(4) 0.71845(15) 0.1366(2) 0.0346(8) Uani 1 1 d . . .
H15 H 0.3819 0.702 0.1023 0.042 Uiso 1 1 calc R . .
C16 C 0.5516(5) 0.67734(17) 0.1799(2) 0.0479(11) Uani 1 1 d . . .
H16 H 0.5376 0.6334 0.1739 0.058 Uiso 1 1 calc R . .
C17 C 0.6635(5) 0.69963(19) 0.2316(2) 0.0506(11) Uani 1 1 d . . .
H17 H 0.7254 0.6714 0.2622 0.061 Uiso 1 1 calc R . .
C18 C 0.6839(4) 0.76355(18) 0.2382(2) 0.0395(9) Uani 1 1 d . . .
H18 H 0.7605 0.7791 0.274 0.047 Uiso 1 1 calc R . .
C19 C 0.5950(3) 0.80602(15) 0.19362(19) 0.0271(7) Uani 1 1 d . . .
C20 C 0.6205(3) 0.87522(15) 0.2053(2) 0.0298(8) Uani 1 1 d . . .
H20A H 0.7194 0.8826 0.2261 0.036 Uiso 1 1 calc R . .
H20B H 0.5992 0.8971 0.1529 0.036 Uiso 1 1 calc R . .
C21 C 0.1994(4) 0.8622(2) -0.0453(2) 0.0496(10) Uani 1 1 d . . .
H21A H 0.1303 0.8312 -0.0339 0.074 Uiso 1 1 calc R . .
H21B H 0.1955 0.8672 -0.1037 0.074 Uiso 1 1 calc R . .
H21C H 0.1796 0.9026 -0.0212 0.074 Uiso 1 1 calc R . .
C22 C 0.5041(4) 0.89577(19) -0.0249(2) 0.0501(10) Uani 1 1 d . . .
H22A H 0.5982 0.8829 -0.0023 0.075 Uiso 1 1 calc R . .
H22B H 0.4822 0.9359 -0.0011 0.075 Uiso 1 1 calc R . .
H22C H 0.4986 0.9004 -0.0834 0.075 Uiso 1 1 calc R . .
C23 C 0.4180(4) 0.76221(18) -0.0562(2) 0.0416(9) Uani 1 1 d . . .
H23A H 0.5105 0.747 -0.034 0.062 Uiso 1 1 calc R . .
H23B H 0.416 0.7718 -0.1136 0.062 Uiso 1 1 calc R . .
H23C H 0.3489 0.7298 -0.0498 0.062 Uiso 1 1 calc R . .
C24 C 0.4678(4) 0.99647(18) 0.3747(2) 0.0445(10) Uani 1 1 d . . .
H24A H 0.4438 0.9634 0.411 0.067 Uiso 1 1 calc R . .
H24B H 0.3846 1.009 0.3384 0.067 Uiso 1 1 calc R . .
H24C H 0.505 1.0328 0.4064 0.067 Uiso 1 1 calc R . .
C25 C 0.7665(4) 0.94979(19) 0.3834(2) 0.0458(10) Uani 1 1 d . . .
H25A H 0.7503 0.9158 0.4204 0.069 Uiso 1 1 calc R . .
H25B H 0.7955 0.9877 0.4144 0.069 Uiso 1 1 calc R . .
H25C H 0.8394 0.9373 0.3517 0.069 Uiso 1 1 calc R . .
C26 C 0.6432(4) 1.03083(17) 0.2460(2) 0.0423(9) Uani 1 1 d . . .
H26A H 0.5603 1.0412 0.2082 0.064 Uiso 1 1 calc R . .
H26B H 0.7175 1.0173 0.2158 0.064 Uiso 1 1 calc R . .
H26C H 0.6735 1.0679 0.2783 0.064 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
Li1 0.025(3) 0.033(3) 0.031(3) 0.000(2) 0.006(2) -0.001(2)
Li2 0.031(3) 0.029(3) 0.036(3) 0.003(2) 0.006(2) 0.001(2)
Li3 0.026(3) 0.027(3) 0.032(3) -0.002(2) 0.002(2) 0.000(2)
Li4 0.028(3) 0.036(3) 0.039(3) -0.006(3) 0.009(3) -0.003(2)
Si1 0.0254(5) 0.0457(6) 0.0248(5) 0.0058(4) 0.0007(4) -0.0067(4)
Si2 0.0239(5) 0.0237(5) 0.0328(5) 0.0025(4) 0.0036(4) 0.0044(4)
Si3 0.0293(5) 0.0337(5) 0.0243(5) -0.0002(4) 0.0024(4) 0.0037(4)
Si4 0.0267(5) 0.0279(5) 0.0338(5) -0.0014(4) 0.0021(4) -0.0068(4)
N1 0.0229(14) 0.0266(14) 0.0262(14) 0.0026(12) 0.0043(11) -0.0026(11)
N2 0.0208(13) 0.0241(14) 0.0288(14) 0.0033(11) 0.0077(11) 0.0009(11)
N3 0.0245(14) 0.0256(15) 0.0246(14) 0.0016(11) 0.0057(11) 0.0019(11)
N4 0.0210(13) 0.0253(14) 0.0283(14) -0.0006(11) 0.0031(11) -0.0028(11)
C1 0.0258(17) 0.0270(18) 0.0227(16) 0.0047(13) 0.0073(13) -0.0031(14)
C2 0.044(2) 0.0287(19) 0.036(2) 0.0053(15) 0.0090(17) 0.0019(16)
C3 0.073(3) 0.0254(19) 0.047(2) -0.0021(17) 0.017(2) -0.012(2)
C4 0.066(3) 0.043(2) 0.035(2) -0.0048(18) 0.009(2) -0.026(2)
C5 0.034(2) 0.052(2) 0.0283(19) 0.0055(17) 0.0008(15) -0.0122(18)
C6 0.0234(16) 0.0319(18) 0.0243(17) 0.0049(14) 0.0059(13) -0.0060(14)
C7 0.0209(16) 0.0359(19) 0.0310(19) 0.0041(15) 0.0070(14) 0.0037(14)
C8 0.054(2) 0.063(3) 0.037(2) -0.010(2) 0.0171(19) -0.011(2)
C9 0.033(2) 0.072(3) 0.035(2) 0.007(2) -0.0024(16) -0.015(2)
C10 0.039(2) 0.062(3) 0.039(2) 0.022(2) -0.0014(17) -0.012(2)
C11 0.041(2) 0.036(2) 0.051(2) -0.0047(18) 0.0139(18) 0.0084(17)
C12 0.0311(19) 0.040(2) 0.045(2) 0.0086(17) -0.0007(16) 0.0066(16)
C13 0.034(2) 0.0288(19) 0.047(2) 0.0065(16) 0.0043(17) -0.0008(15)
C14 0.0326(18) 0.0246(17) 0.0222(16) 0.0036(13) 0.0112(14) 0.0040(14)
C15 0.047(2) 0.0266(18) 0.0327(19) 0.0006(15) 0.0155(17) 0.0013(16)
C16 0.080(3) 0.024(2) 0.047(2) 0.0112(17) 0.034(2) 0.014(2)
C17 0.072(3) 0.049(3) 0.034(2) 0.0141(19) 0.015(2) 0.035(2)
C18 0.036(2) 0.053(2) 0.0299(19) 0.0037(17) 0.0070(16) 0.0224(18)
C19 0.0280(17) 0.0294(18) 0.0253(17) 0.0009(14) 0.0090(14) 0.0091(14)
C20 0.0208(16) 0.038(2) 0.0308(19) -0.0007(15) 0.0042(14) -0.0025(14)
C21 0.049(2) 0.055(3) 0.041(2) -0.0012(19) -0.0048(19) 0.018(2)
C22 0.064(3) 0.048(2) 0.040(2) 0.0094(19) 0.016(2) -0.004(2)
C23 0.041(2) 0.052(2) 0.031(2) -0.0080(18) 0.0041(16) 0.0067(18)
C24 0.044(2) 0.041(2) 0.049(2) -0.0151(18) 0.0077(18) -0.0053(18)
C25 0.038(2) 0.054(3) 0.043(2) 0.0007(19) -0.0031(17) -0.0136(19)
C26 0.042(2) 0.031(2) 0.054(2) 0.0059(18) 0.0075(18) -0.0075(17)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_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
Li1 N2 2.016(6) . ?
Li1 N1 2.031(6) . ?
Li1 N4 2.074(6) . ?
Li1 Li3 2.368(8) . ?
Li2 N1 1.945(6) . ?
Li2 N4 2.040(6) . ?
Li2 C19 2.314(6) . ?
Li3 N3 2.026(6) . ?
Li3 N4 2.050(6) . ?
Li3 N2 2.083(6) . ?
Li4 N3 1.943(6) . ?
Li4 N2 2.040(6) . ?
Li4 C6 2.354(7) . ?
Si1 N1 1.702(3) . ?
Si1 C8 1.868(4) . ?
Si1 C10 1.870(4) . ?
Si1 C9 1.875(3) . ?
Si2 N2 1.711(3) . ?
Si2 C11 1.862(4) . ?
Si2 C13 1.870(3) . ?
Si2 C12 1.871(3) . ?
Si3 N3 1.709(3) . ?
Si3 C23 1.872(4) . ?
Si3 C22 1.872(4) . ?
Si3 C21 1.876(4) . ?
Si4 N4 1.716(3) . ?
Si4 C26 1.863(4) . ?
Si4 C24 1.876(4) . ?
Si4 C25 1.880(4) . ?
N1 C1 1.405(4) . ?
N2 C7 1.491(4) . ?
N3 C14 1.413(4) . ?
N4 C20 1.502(4) . ?
C1 C2 1.401(5) . ?
C1 C6 1.423(4) . ?
C2 C3 1.378(5) . ?
C2 H2 0.95 . ?
C3 C4 1.373(6) . ?
C3 H3 0.95 . ?
C4 C5 1.376(5) . ?
C4 H4 0.95 . ?
C5 C6 1.392(5) . ?
C5 H5 0.95 . ?
C6 C7 1.504(5) . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.400(4) . ?
C14 C19 1.421(4) . ?
C15 C16 1.385(5) . ?
C15 H15 0.95 . ?
C16 C17 1.379(6) . ?
C16 H16 0.95 . ?
C17 C18 1.379(6) . ?
C17 H17 0.95 . ?
C18 C19 1.395(4) . ?
C18 H18 0.95 . ?
C19 C20 1.504(4) . ?
C20 H20A 0.99 . ?
C20 H20B 0.99 . ?
C21 H21A 0.98 . ?
C21 H21B 0.98 . ?
C21 H21C 0.98 . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 H23A 0.98 . ?
C23 H23B 0.98 . ?
C23 H23C 0.98 . ?
C24 H24A 0.98 . ?
C24 H24B 0.98 . ?
C24 H24C 0.98 . ?
C25 H25A 0.98 . ?
C25 H25B 0.98 . ?
C25 H25C 0.98 . ?
C26 H26A 0.98 . ?
C26 H26B 0.98 . ?
C26 H26C 0.98 . ?
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 Li1 N1 109.0(3) . . ?
N2 Li1 N4 110.5(3) . . ?
N1 Li1 N4 104.6(3) . . ?
N2 Li1 Li3 56.0(2) . . ?
N1 Li1 Li3 120.7(3) . . ?
N4 Li1 Li3 54.47(19) . . ?
N1 Li2 N4 109.2(3) . . ?
N1 Li2 C19 137.0(3) . . ?
N4 Li2 C19 68.6(2) . . ?
N1 Li2 Li1 54.4(2) . . ?
N4 Li2 Li1 54.8(2) . . ?
C19 Li2 Li1 107.6(3) . . ?
N3 Li3 N4 110.4(3) . . ?
N3 Li3 N2 104.1(3) . . ?
N4 Li3 N2 108.8(3) . . ?
N3 Li3 Li1 120.8(3) . . ?
N4 Li3 Li1 55.4(2) . . ?
N2 Li3 Li1 53.40(19) . . ?
N3 Li4 N2 108.9(3) . . ?
N3 Li4 C6 140.8(3) . . ?
N2 Li4 C6 68.2(2) . . ?
N3 Li4 Li3 54.0(2) . . ?
N2 Li4 Li3 54.9(2) . . ?
C6 Li4 Li3 109.1(3) . . ?
N1 Si1 C8 112.41(16) . . ?
N1 Si1 C10 114.82(16) . . ?
C8 Si1 C10 106.25(19) . . ?
N1 Si1 C9 106.63(15) . . ?
C8 Si1 C9 107.55(19) . . ?
C10 Si1 C9 108.95(18) . . ?
N2 Si2 C11 113.95(15) . . ?
N2 Si2 C13 106.26(14) . . ?
C11 Si2 C13 107.92(17) . . ?
N2 Si2 C12 113.69(15) . . ?
C11 Si2 C12 106.05(17) . . ?
C13 Si2 C12 108.78(17) . . ?
N3 Si3 C23 114.46(15) . . ?
N3 Si3 C22 111.98(16) . . ?
C23 Si3 C22 106.17(18) . . ?
N3 Si3 C21 108.30(16) . . ?
C23 Si3 C21 108.15(18) . . ?
C22 Si3 C21 107.51(19) . . ?
N4 Si4 C26 114.04(15) . . ?
N4 Si4 C24 106.28(15) . . ?
C26 Si4 C24 107.56(18) . . ?
N4 Si4 C25 113.67(16) . . ?
C26 Si4 C25 106.18(17) . . ?
C24 Si4 C25 108.89(18) . . ?
C1 N1 Si1 121.0(2) . . ?
C1 N1 Li2 112.6(3) . . ?
Si1 N1 Li2 112.7(2) . . ?
C1 N1 Li1 109.2(2) . . ?
Si1 N1 Li1 117.8(2) . . ?
Li2 N1 Li1 74.5(2) . . ?
C7 N2 Si2 113.80(19) . . ?
C7 N2 Li1 88.3(2) . . ?
Si2 N2 Li1 123.9(2) . . ?
C7 N2 Li4 92.7(2) . . ?
Si2 N2 Li4 122.1(2) . . ?
Li1 N2 Li4 106.4(2) . . ?
C7 N2 Li3 148.1(2) . . ?
Si2 N2 Li3 97.93(19) . . ?
Li1 N2 Li3 70.6(2) . . ?
Li4 N2 Li3 71.8(2) . . ?
C14 N3 Si3 118.8(2) . . ?
C14 N3 Li4 108.1(3) . . ?
Si3 N3 Li4 121.0(2) . . ?
C14 N3 Li3 107.6(2) . . ?
Si3 N3 Li3 118.1(2) . . ?
Li4 N3 Li3 75.0(2) . . ?
C20 N4 Si4 112.65(19) . . ?
C20 N4 Li2 92.1(2) . . ?
Si4 N4 Li2 123.0(2) . . ?
C20 N4 Li3 86.6(2) . . ?
Si4 N4 Li3 124.7(2) . . ?
Li2 N4 Li3 106.4(2) . . ?
C20 N4 Li1 145.5(2) . . ?
Si4 N4 Li1 101.6(2) . . ?
Li2 N4 Li1 71.7(2) . . ?
Li3 N4 Li1 70.1(2) . . ?
C2 C1 N1 122.2(3) . . ?
C2 C1 C6 116.4(3) . . ?
N1 C1 C6 121.5(3) . . ?
C3 C2 C1 122.7(3) . . ?
C3 C2 H2 118.7 . . ?
C1 C2 H2 118.7 . . ?
C4 C3 C2 120.3(4) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C3 C4 C5 118.9(4) . . ?
C3 C4 H4 120.5 . . ?
C5 C4 H4 120.5 . . ?
C4 C5 C6 122.1(3) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 119.6(3) . . ?
C5 C6 C7 119.9(3) . . ?
C1 C6 C7 120.4(3) . . ?
C5 C6 Li4 84.8(2) . . ?
C1 C6 Li4 101.9(2) . . ?
C7 C6 Li4 80.8(2) . . ?
N2 C7 C6 111.5(2) . . ?
N2 C7 H7A 109.3 . . ?
C6 C7 H7A 109.3 . . ?
N2 C7 H7B 109.3 . . ?
C6 C7 H7B 109.3 . . ?
H7A C7 H7B 108 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C15 C14 N3 121.4(3) . . ?
C15 C14 C19 117.0(3) . . ?
N3 C14 C19 121.5(3) . . ?
C16 C15 C14 121.9(4) . . ?
C16 C15 H15 119 . . ?
C14 C15 H15 119 . . ?
C17 C16 C15 120.6(4) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C16 C17 C18 118.9(3) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C17 C18 C19 121.8(4) . . ?
C17 C18 H18 119.1 . . ?
C19 C18 H18 119.1 . . ?
C18 C19 C14 119.7(3) . . ?
C18 C19 C20 119.2(3) . . ?
C14 C19 C20 121.0(3) . . ?
C18 C19 Li2 80.0(2) . . ?
C14 C19 Li2 104.8(2) . . ?
C20 C19 Li2 81.9(2) . . ?
N4 C20 C19 110.2(3) . . ?
N4 C20 Li3 55.96(19) . . ?
C19 C20 Li3 93.7(2) . . ?
N4 C20 H20A 109.6 . . ?
C19 C20 H20A 109.6 . . ?
Li3 C20 H20A 156.3 . . ?
N4 C20 H20B 109.6 . . ?
C19 C20 H20B 109.6 . . ?
Li3 C20 H20B 65.9 . . ?
H20A C20 H20B 108.1 . . ?
Si3 C21 H21A 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
Si3 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si4 C25 H25A 109.5 . . ?
Si4 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
Si4 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
Si4 C26 H26A 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
#===END
data_(4b)-dec1496
_database_code_depnum_ccdc_archive 'CCDC 819595'
#TrackingRef '- Combined_cif.cif'
_audit_creation_date 2011-03-17T09:56:53-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.2
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C34 H64 Li4 N4 O2 Si4'
_chemical_formula_sum 'C34 H64 Li4 N4 O2 Si4'
_chemical_formula_weight 701.01
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting monoclinic
_symmetry_space_group_name_H-M P2(1)/c
_symmetry_space_group_name_Hall '-P 2ybc'
_symmetry_Int_Tables_number 14
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
_cell_length_a 19.787(7)
_cell_length_b 9.808(3)
_cell_length_c 21.951(9)
_cell_angle_alpha 90.00(3)
_cell_angle_beta 99.70(3)
_cell_angle_gamma 90.00(2)
_cell_volume 4199(3)
_cell_formula_units_Z 4
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 7
_cell_measurement_theta_max 10
_cell_measurement_wavelength 0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description Block
_exptl_crystal_colour Colourless
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.4
_exptl_crystal_density_diffrn 1.109
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 1520
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 0.174
_exptl_absorpt_correction_type none
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.7107
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_measurement_device 'Enraf-Nonius CAD4'
_diffrn_measurement_method 'omega-2theta scans'
_diffrn_standards_number ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_av_R_equivalents 0.0693
_diffrn_reflns_av_unetI/netI 0.08
_diffrn_reflns_number 5315
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 20
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_limit_l_max 22
_diffrn_reflns_theta_min 2.09
_diffrn_reflns_theta_max 21.99
_diffrn_reflns_theta_full 21.99
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total 5146
_reflns_number_gt 3736
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'Enraf-Nonius CAD4 software'
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;
One of the methylene groups on THF is disordered and was refined with bond
restraints (SADI)
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^)+(0.0663P)^2^+2.3296P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 5146
_refine_ls_number_parameters 443
_refine_ls_number_restraints 2
_refine_ls_R_factor_all 0.0855
_refine_ls_R_factor_gt 0.0556
_refine_ls_wR_factor_ref 0.15
_refine_ls_wR_factor_gt 0.1322
_refine_ls_goodness_of_fit_ref 1.026
_refine_ls_restrained_S_all 1.026
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.265
_refine_diff_density_min -0.29
_refine_diff_density_rms 0.062
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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 0 '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 0.006 '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'
Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.07770(6) 0.35182(13) 0.70901(6) 0.0289(3) Uani 1 1 d . B .
Si2 Si 0.36397(6) 0.51610(12) 0.73074(5) 0.0280(3) Uani 1 1 d . B .
Si3 Si 0.42043(6) 0.23072(13) 0.55312(6) 0.0297(3) Uani 1 1 d . B .
Si4 Si 0.28576(6) 0.06212(13) 0.76339(5) 0.0289(3) Uani 1 1 d . B .
O1 O 0.09508(14) -0.0172(3) 0.63723(13) 0.0328(8) Uani 1 1 d . . .
O2 O 0.33817(15) 0.5937(3) 0.53021(13) 0.0342(8) Uani 1 1 d . . .
N1 N 0.13926(16) 0.3261(3) 0.66488(15) 0.0236(8) Uani 1 1 d . . .
N2 N 0.29811(16) 0.4579(3) 0.67630(14) 0.0224(8) Uani 1 1 d . . .
N3 N 0.34218(16) 0.2527(3) 0.57469(14) 0.0235(8) Uani 1 1 d . . .
N4 N 0.26992(16) 0.1213(3) 0.68938(14) 0.0221(8) Uani 1 1 d . . .
C1 C 0.13937(19) 0.4048(4) 0.61123(18) 0.0231(10) Uani 1 1 d . B .
C2 C 0.0929(2) 0.3771(4) 0.55647(19) 0.0303(11) Uani 1 1 d . . .
H2 H 0.0607 0.3055 0.5569 0.036 Uiso 1 1 calc R B .
C3 C 0.0920(2) 0.4483(5) 0.5027(2) 0.0371(12) Uani 1 1 d . B .
H3 H 0.0599 0.4249 0.467 0.045 Uiso 1 1 calc R . .
C4 C 0.1372(2) 0.5532(5) 0.5001(2) 0.0373(12) Uani 1 1 d . . .
H4 H 0.1366 0.6036 0.463 0.045 Uiso 1 1 calc R B .
C5 C 0.1841(2) 0.5842(5) 0.55310(19) 0.0300(11) Uani 1 1 d . B .
H5 H 0.2156 0.6568 0.5517 0.036 Uiso 1 1 calc R . .
C6 C 0.18625(19) 0.5122(4) 0.60820(18) 0.0215(10) Uani 1 1 d . . .
C7 C 0.23856(19) 0.5529(4) 0.66323(18) 0.0223(10) Uani 1 1 d . B .
H7B H 0.2557 0.6454 0.656 0.027 Uiso 1 1 calc R . .
H7A H 0.2159 0.5574 0.7001 0.027 Uiso 1 1 calc R . .
C8 C 0.0958(2) 0.5031(5) 0.7614(2) 0.0420(13) Uani 1 1 d . . .
H8C H 0.0594 0.5123 0.7863 0.063 Uiso 1 1 calc R B .
H8B H 0.0976 0.5856 0.7366 0.063 Uiso 1 1 calc R . .
H8A H 0.1399 0.4903 0.7887 0.063 Uiso 1 1 calc R . .
C9 C -0.0110(2) 0.3755(5) 0.6644(2) 0.0424(13) Uani 1 1 d . . .
H9C H -0.0246 0.2937 0.6397 0.064 Uiso 1 1 calc R B .
H9B H -0.0116 0.4545 0.6369 0.064 Uiso 1 1 calc R . .
H9A H -0.0431 0.3908 0.6932 0.064 Uiso 1 1 calc R . .
C10 C 0.0752(2) 0.2004(5) 0.7601(2) 0.0414(13) Uani 1 1 d . . .
H10C H 0.1195 0.1907 0.7874 0.062 Uiso 1 1 calc R B .
H10B H 0.0657 0.1183 0.7347 0.062 Uiso 1 1 calc R . .
H10A H 0.039 0.2128 0.7851 0.062 Uiso 1 1 calc R . .
C11 C 0.3368(2) 0.5767(5) 0.8035(2) 0.0422(13) Uani 1 1 d . . .
H11C H 0.3774 0.5984 0.8341 0.063 Uiso 1 1 calc R B .
H11B H 0.3103 0.505 0.8198 0.063 Uiso 1 1 calc R . .
H11A H 0.3083 0.6585 0.7949 0.063 Uiso 1 1 calc R . .
C12 C 0.4259(2) 0.3718(5) 0.7500(2) 0.0401(12) Uani 1 1 d . . .
H12C H 0.4448 0.3461 0.7131 0.06 Uiso 1 1 calc R B .
H12B H 0.4021 0.2935 0.7643 0.06 Uiso 1 1 calc R . .
H12A H 0.4633 0.4004 0.7827 0.06 Uiso 1 1 calc R . .
C13 C 0.4136(2) 0.6596(5) 0.7041(2) 0.0410(13) Uani 1 1 d . . .
H13C H 0.3843 0.7404 0.6966 0.062 Uiso 1 1 calc R B .
H13B H 0.4294 0.6335 0.6657 0.062 Uiso 1 1 calc R . .
H13A H 0.4533 0.6802 0.7359 0.062 Uiso 1 1 calc R . .
C14 C 0.2867(2) 0.1705(4) 0.54575(18) 0.0244(10) Uani 1 1 d . B .
C15 C 0.2544(2) 0.1953(5) 0.48528(18) 0.0290(11) Uani 1 1 d . . .
H15 H 0.27 0.2697 0.4636 0.035 Uiso 1 1 calc R B .
C16 C 0.2014(2) 0.1182(5) 0.4556(2) 0.0407(13) Uani 1 1 d . B .
H16 H 0.1815 0.139 0.4142 0.049 Uiso 1 1 calc R . .
C17 C 0.1769(2) 0.0106(5) 0.4855(2) 0.0376(12) Uani 1 1 d . . .
H17 H 0.1406 -0.0444 0.4651 0.045 Uiso 1 1 calc R B .
C18 C 0.2066(2) -0.0158(4) 0.5463(2) 0.0315(11) Uani 1 1 d . B .
H18 H 0.1893 -0.0889 0.5675 0.038 Uiso 1 1 calc R . .
C19 C 0.2609(2) 0.0614(4) 0.57726(18) 0.0230(10) Uani 1 1 d . . .
C20 C 0.2903(2) 0.0247(4) 0.64320(18) 0.0263(10) Uani 1 1 d . B .
H20B H 0.2748 -0.0682 0.652 0.032 Uiso 1 1 calc R . .
H20A H 0.341 0.023 0.6479 0.032 Uiso 1 1 calc R . .
C21 C 0.4755(2) 0.3815(5) 0.5799(2) 0.0447(13) Uani 1 1 d . . .
H21C H 0.522 0.3662 0.5713 0.067 Uiso 1 1 calc R B .
H21B H 0.4774 0.3941 0.6244 0.067 Uiso 1 1 calc R . .
H21A H 0.4561 0.4633 0.5579 0.067 Uiso 1 1 calc R . .
C22 C 0.4657(2) 0.0762(5) 0.5905(2) 0.0495(14) Uani 1 1 d . . .
H22C H 0.4408 -0.0061 0.5745 0.074 Uiso 1 1 calc R B .
H22B H 0.4675 0.0812 0.6354 0.074 Uiso 1 1 calc R . .
H22A H 0.5124 0.0729 0.5813 0.074 Uiso 1 1 calc R . .
C23 C 0.4193(2) 0.2128(5) 0.4681(2) 0.0448(13) Uani 1 1 d . . .
H23C H 0.4003 0.2959 0.447 0.067 Uiso 1 1 calc R B .
H23B H 0.3907 0.1346 0.4524 0.067 Uiso 1 1 calc R . .
H23A H 0.4661 0.1986 0.4604 0.067 Uiso 1 1 calc R . .
C24 C 0.2712(2) 0.2063(5) 0.81574(19) 0.0384(12) Uani 1 1 d . . .
H24C H 0.2231 0.2354 0.8063 0.058 Uiso 1 1 calc R B .
H24B H 0.301 0.283 0.8095 0.058 Uiso 1 1 calc R . .
H24A H 0.2817 0.1761 0.8588 0.058 Uiso 1 1 calc R . .
C25 C 0.2268(2) -0.0780(5) 0.7788(2) 0.0400(12) Uani 1 1 d . . .
H25C H 0.2357 -0.1596 0.7557 0.06 Uiso 1 1 calc R B .
H25B H 0.1791 -0.0491 0.7658 0.06 Uiso 1 1 calc R . .
H25A H 0.2346 -0.0987 0.8231 0.06 Uiso 1 1 calc R . .
C26 C 0.3751(2) -0.0022(5) 0.7896(2) 0.0401(12) Uani 1 1 d . . .
H26C H 0.3815 -0.0237 0.8338 0.06 Uiso 1 1 calc R B .
H26B H 0.4081 0.0681 0.7825 0.06 Uiso 1 1 calc R . .
H26A H 0.3825 -0.0845 0.7664 0.06 Uiso 1 1 calc R . .
C30 C 0.0979(2) -0.1583(4) 0.6553(2) 0.0378(12) Uani 1 1 d . B .
H30B H 0.0876 -0.1681 0.6977 0.045 Uiso 1 1 calc R A 1
H30A H 0.1441 -0.1961 0.6544 0.045 Uiso 1 1 calc R A 1
C31 C 0.3614(3) 0.7312(5) 0.5445(2) 0.0417(13) Uani 1 1 d . . .
H31B H 0.4105 0.7313 0.5634 0.05 Uiso 1 1 calc R . .
H31A H 0.3348 0.7734 0.5739 0.05 Uiso 1 1 calc R . .
C32 C 0.3510(2) 0.8091(5) 0.4845(2) 0.0416(12) Uani 1 1 d . . .
H32B H 0.3336 0.9022 0.49 0.05 Uiso 1 1 calc R . .
H32A H 0.3941 0.8154 0.4675 0.05 Uiso 1 1 calc R . .
C33 C 0.2986(3) 0.7251(5) 0.4436(2) 0.0515(14) Uani 1 1 d . . .
H33B H 0.2515 0.7492 0.4494 0.062 Uiso 1 1 calc R . .
H33A H 0.3024 0.737 0.3995 0.062 Uiso 1 1 calc R . .
C34 C 0.3164(3) 0.5829(5) 0.4647(2) 0.0481(14) Uani 1 1 d . . .
H34B H 0.276 0.5223 0.455 0.058 Uiso 1 1 calc R . .
H34A H 0.3537 0.5463 0.4445 0.058 Uiso 1 1 calc R . .
Li1 Li 0.2361(3) 0.3125(7) 0.7031(3) 0.0295(17) Uani 1 1 d . B .
Li2 Li 0.3326(4) 0.2655(8) 0.6615(3) 0.0318(18) Uani 1 1 d . B .
Li3 Li 0.1646(3) 0.1296(7) 0.6501(3) 0.0311(17) Uani 1 1 d . B .
Li4 Li 0.3151(4) 0.4470(7) 0.5847(3) 0.0316(18) Uani 1 1 d . B .
C27 C 0.0349(2) 0.0020(5) 0.5917(2) 0.0483(14) Uani 0.438(18) 1 d PD B 1
H27A H 0.0423 0.0735 0.5617 0.058 Uiso 0.438(18) 1 calc PR B 1
H27B H -0.0048 0.028 0.6113 0.058 Uiso 0.438(18) 1 calc PR B 1
C28 C 0.0233(9) -0.1363(10) 0.5602(6) 0.042(5) Uani 0.438(18) 1 d PD B 1
H28A H -0.0256 -0.1495 0.5423 0.051 Uiso 0.438(18) 1 calc PR B 1
H28B H 0.0513 -0.1459 0.5271 0.051 Uiso 0.438(18) 1 calc PR B 1
C29 C 0.0450(2) -0.2317(5) 0.6096(2) 0.0464(13) Uani 0.438(18) 1 d PD B 1
H29A H 0.065 -0.3142 0.5937 0.056 Uiso 0.438(18) 1 calc PR B 1
H29B H 0.0056 -0.2595 0.6293 0.056 Uiso 0.438(18) 1 calc PR B 1
C27A C 0.0349(2) 0.0020(5) 0.5917(2) 0.0483(14) Uani 0.562(18) 1 d PD B 2
H27C H 0.0476 0.0182 0.5506 0.058 Uiso 0.562(18) 1 calc PR B 2
H27D H 0.0084 0.0814 0.6025 0.058 Uiso 0.562(18) 1 calc PR B 2
C28A C -0.0070(4) -0.1268(8) 0.5910(6) 0.034(3) Uani 0.562(18) 1 d PD B 2
H28C H -0.0395 -0.1209 0.6207 0.041 Uiso 0.562(18) 1 calc PR B 2
H28D H -0.033 -0.1453 0.5492 0.041 Uiso 0.562(18) 1 calc PR B 2
C29A C 0.0450(2) -0.2317(5) 0.6096(2) 0.0464(13) Uani 0.562(18) 1 d PD B 2
H29C H 0.0648 -0.2646 0.5738 0.056 Uiso 0.562(18) 1 calc PR B 2
H29D H 0.0255 -0.3102 0.6292 0.056 Uiso 0.562(18) 1 calc PR B 2
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Si1 0.0224(7) 0.0287(7) 0.0368(8) 0.0047(6) 0.0088(5) 0.0032(6)
Si2 0.0227(7) 0.0271(7) 0.0315(7) -0.0080(6) -0.0037(5) 0.0030(6)
Si3 0.0234(7) 0.0300(8) 0.0365(8) -0.0101(6) 0.0074(5) -0.0007(6)
Si4 0.0312(7) 0.0282(7) 0.0251(7) 0.0026(6) -0.0014(5) 0.0058(6)
O1 0.0302(17) 0.0285(18) 0.0387(18) -0.0005(15) 0.0029(14) -0.0039(14)
O2 0.0388(18) 0.0277(19) 0.0383(19) 0.0016(15) 0.0132(15) -0.0058(15)
N1 0.0212(19) 0.022(2) 0.027(2) 0.0063(16) 0.0027(15) 0.0015(16)
N2 0.0197(18) 0.022(2) 0.0242(19) -0.0065(16) 0.0007(15) 0.0031(16)
N3 0.0217(19) 0.025(2) 0.0231(19) -0.0063(16) 0.0022(15) -0.0010(16)
N4 0.0227(19) 0.0208(19) 0.0224(19) -0.0023(16) 0.0029(15) 0.0063(16)
C1 0.014(2) 0.027(3) 0.028(2) 0.002(2) 0.0022(18) 0.0057(19)
C2 0.025(2) 0.026(3) 0.038(3) 0.001(2) -0.002(2) -0.007(2)
C3 0.033(3) 0.044(3) 0.029(3) 0.004(2) -0.011(2) -0.005(2)
C4 0.036(3) 0.041(3) 0.032(3) 0.011(2) -0.001(2) 0.000(2)
C5 0.024(2) 0.033(3) 0.033(3) 0.006(2) 0.006(2) -0.003(2)
C6 0.016(2) 0.020(2) 0.029(2) 0.001(2) 0.0026(18) 0.0025(19)
C7 0.020(2) 0.017(2) 0.029(2) -0.0026(19) 0.0029(18) 0.0004(19)
C8 0.046(3) 0.044(3) 0.039(3) 0.002(2) 0.017(2) 0.008(3)
C9 0.029(3) 0.048(3) 0.052(3) 0.003(3) 0.010(2) 0.003(2)
C10 0.039(3) 0.041(3) 0.047(3) 0.008(2) 0.016(2) 0.001(2)
C11 0.046(3) 0.039(3) 0.038(3) -0.010(2) -0.004(2) 0.008(2)
C12 0.030(3) 0.044(3) 0.041(3) -0.009(2) -0.007(2) 0.008(2)
C13 0.030(3) 0.041(3) 0.047(3) -0.010(2) -0.006(2) -0.005(2)
C14 0.020(2) 0.026(3) 0.027(2) -0.005(2) 0.0060(19) 0.005(2)
C15 0.031(3) 0.032(3) 0.024(2) 0.002(2) 0.006(2) -0.005(2)
C16 0.031(3) 0.059(4) 0.030(3) -0.001(3) 0.000(2) -0.006(3)
C17 0.029(3) 0.051(3) 0.031(3) -0.009(3) 0.002(2) -0.010(2)
C18 0.031(3) 0.028(3) 0.038(3) -0.003(2) 0.014(2) -0.005(2)
C19 0.021(2) 0.024(2) 0.025(2) -0.007(2) 0.0048(19) 0.003(2)
C20 0.027(2) 0.020(2) 0.031(2) 0.003(2) 0.006(2) 0.003(2)
C21 0.030(3) 0.050(3) 0.055(3) -0.017(3) 0.012(2) -0.008(2)
C22 0.029(3) 0.047(3) 0.073(4) -0.003(3) 0.012(3) 0.009(2)
C23 0.035(3) 0.059(4) 0.046(3) -0.011(3) 0.020(2) 0.002(3)
C24 0.042(3) 0.045(3) 0.027(3) -0.005(2) 0.003(2) 0.004(2)
C25 0.042(3) 0.035(3) 0.041(3) 0.016(2) 0.001(2) 0.006(2)
C26 0.041(3) 0.043(3) 0.033(3) 0.003(2) -0.005(2) 0.015(2)
C30 0.040(3) 0.029(3) 0.042(3) 0.008(2) 0.001(2) -0.003(2)
C31 0.043(3) 0.036(3) 0.047(3) -0.003(3) 0.012(2) -0.006(2)
C32 0.053(3) 0.035(3) 0.041(3) -0.001(2) 0.020(2) -0.009(3)
C33 0.076(4) 0.038(3) 0.039(3) 0.004(3) 0.006(3) -0.019(3)
C34 0.074(4) 0.038(3) 0.037(3) -0.011(2) 0.024(3) -0.015(3)
Li1 0.021(4) 0.029(4) 0.037(4) -0.007(3) 0.000(3) 0.004(3)
Li2 0.031(4) 0.034(5) 0.032(4) -0.004(3) 0.010(3) -0.005(3)
Li3 0.026(4) 0.030(4) 0.037(4) -0.003(4) 0.002(3) 0.004(3)
Li4 0.032(4) 0.029(4) 0.035(4) -0.004(3) 0.010(3) 0.001(3)
C27 0.040(3) 0.036(3) 0.062(4) 0.009(3) -0.011(3) -0.005(3)
C28 0.043(9) 0.043(8) 0.037(8) 0.006(6) -0.004(6) -0.020(7)
C29 0.040(3) 0.038(3) 0.056(3) -0.004(3) -0.004(3) -0.005(3)
C27A 0.040(3) 0.036(3) 0.062(4) 0.009(3) -0.011(3) -0.005(3)
C28A 0.024(5) 0.035(5) 0.043(7) -0.002(5) 0.002(4) -0.006(4)
C29A 0.040(3) 0.038(3) 0.056(3) -0.004(3) -0.004(3) -0.005(3)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Si1 N1 1.698(3) . ?
Si1 C10 1.867(5) . ?
Si1 C8 1.874(5) . ?
Si1 C9 1.874(4) . ?
Si2 N2 1.711(3) . ?
Si2 C13 1.866(5) . ?
Si2 C11 1.867(5) . ?
Si2 C12 1.874(4) . ?
Si3 N3 1.707(3) . ?
Si3 C23 1.871(5) . ?
Si3 C21 1.873(5) . ?
Si3 C22 1.878(5) . ?
Si4 N4 1.704(3) . ?
Si4 C25 1.870(5) . ?
Si4 C26 1.874(4) . ?
Si4 C24 1.875(4) . ?
O1 C27 1.433(5) . ?
O1 C30 1.438(5) . ?
O1 Li3 1.979(8) . ?
O2 C34 1.434(5) . ?
O2 C31 1.442(5) . ?
O2 Li4 1.973(8) . ?
N1 C1 1.409(5) . ?
N1 Li1 1.963(7) . ?
N1 Li3 2.032(8) . ?
N2 C7 1.492(5) . ?
N2 Li1 2.032(8) . ?
N2 Li2 2.051(8) . ?
N2 Li4 2.096(8) . ?
N3 C14 1.423(5) . ?
N3 Li2 1.950(8) . ?
N3 Li4 2.002(8) . ?
N4 C20 1.492(5) . ?
N4 Li1 2.030(8) . ?
N4 Li2 2.041(8) . ?
N4 Li3 2.118(7) . ?
C1 C2 1.411(5) . ?
C1 C6 1.412(5) . ?
C2 C3 1.368(6) . ?
C2 H2 0.95 . ?
C3 C4 1.371(6) . ?
C3 H3 0.95 . ?
C4 C5 1.393(6) . ?
C4 H4 0.95 . ?
C5 C6 1.395(6) . ?
C5 H5 0.95 . ?
C6 C7 1.506(5) . ?
C7 H7B 0.99 . ?
C7 H7A 0.99 . ?
C8 H8C 0.98 . ?
C8 H8B 0.98 . ?
C8 H8A 0.98 . ?
C9 H9C 0.98 . ?
C9 H9B 0.98 . ?
C9 H9A 0.98 . ?
C10 H10C 0.98 . ?
C10 H10B 0.98 . ?
C10 H10A 0.98 . ?
C11 H11C 0.98 . ?
C11 H11B 0.98 . ?
C11 H11A 0.98 . ?
C12 H12C 0.98 . ?
C12 H12B 0.98 . ?
C12 H12A 0.98 . ?
C13 H13C 0.98 . ?
C13 H13B 0.98 . ?
C13 H13A 0.98 . ?
C14 C15 1.394(5) . ?
C14 C19 1.414(6) . ?
C15 C16 1.365(6) . ?
C15 H15 0.95 . ?
C16 C17 1.373(6) . ?
C16 H16 0.95 . ?
C17 C18 1.389(6) . ?
C17 H17 0.95 . ?
C18 C19 1.394(6) . ?
C18 H18 0.95 . ?
C19 C20 1.510(5) . ?
C20 H20B 0.99 . ?
C20 H20A 0.99 . ?
C21 H21C 0.98 . ?
C21 H21B 0.98 . ?
C21 H21A 0.98 . ?
C22 H22C 0.98 . ?
C22 H22B 0.98 . ?
C22 H22A 0.98 . ?
C23 H23C 0.98 . ?
C23 H23B 0.98 . ?
C23 H23A 0.98 . ?
C24 H24C 0.98 . ?
C24 H24B 0.98 . ?
C24 H24A 0.98 . ?
C25 H25C 0.98 . ?
C25 H25B 0.98 . ?
C25 H25A 0.98 . ?
C26 H26C 0.98 . ?
C26 H26B 0.98 . ?
C26 H26A 0.98 . ?
C30 C29 1.507(6) . ?
C30 H30B 0.99 . ?
C30 H30A 0.99 . ?
C31 C32 1.506(6) . ?
C31 H31B 0.99 . ?
C31 H31A 0.99 . ?
C32 C33 1.500(6) . ?
C32 H32B 0.99 . ?
C32 H32A 0.99 . ?
C33 C34 1.493(7) . ?
C33 H33B 0.99 . ?
C33 H33A 0.99 . ?
C34 H34B 0.99 . ?
C34 H34A 0.99 . ?
Li1 Li2 2.297(10) . ?
Li1 Li3 2.454(10) . ?
Li2 Li4 2.436(10) . ?
C27 C28 1.522(11) . ?
C27 H27A 0.99 . ?
C27 H27B 0.99 . ?
C28 C29 1.442(11) . ?
C28 H28A 0.99 . ?
C28 H28B 0.99 . ?
C29 H29A 0.99 . ?
C29 H29B 0.99 . ?
C28A H28C 0.99 . ?
C28A H28D 0.99 . ?
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 Si1 C10 108.60(19) . . ?
N1 Si1 C8 112.71(19) . . ?
C10 Si1 C8 106.4(2) . . ?
N1 Si1 C9 114.76(19) . . ?
C10 Si1 C9 107.2(2) . . ?
C8 Si1 C9 106.7(2) . . ?
N2 Si2 C13 114.34(19) . . ?
N2 Si2 C11 114.11(19) . . ?
C13 Si2 C11 105.7(2) . . ?
N2 Si2 C12 107.34(19) . . ?
C13 Si2 C12 106.3(2) . . ?
C11 Si2 C12 108.6(2) . . ?
N3 Si3 C23 115.41(19) . . ?
N3 Si3 C21 108.70(19) . . ?
C23 Si3 C21 107.2(2) . . ?
N3 Si3 C22 111.6(2) . . ?
C23 Si3 C22 106.6(2) . . ?
C21 Si3 C22 106.9(2) . . ?
N4 Si4 C25 113.77(19) . . ?
N4 Si4 C26 114.86(19) . . ?
C25 Si4 C26 106.4(2) . . ?
N4 Si4 C24 107.73(19) . . ?
C25 Si4 C24 106.1(2) . . ?
C26 Si4 C24 107.5(2) . . ?
C27 O1 C30 108.0(3) . . ?
C27 O1 Li3 118.7(3) . . ?
C30 O1 Li3 131.8(3) . . ?
C34 O2 C31 108.5(3) . . ?
C34 O2 Li4 119.6(3) . . ?
C31 O2 Li4 130.4(3) . . ?
C1 N1 Si1 119.9(3) . . ?
C1 N1 Li1 104.8(3) . . ?
Si1 N1 Li1 120.6(3) . . ?
C1 N1 Li3 110.6(3) . . ?
Si1 N1 Li3 116.9(3) . . ?
Li1 N1 Li3 75.8(3) . . ?
C7 N2 Si2 114.2(2) . . ?
C7 N2 Li1 89.9(3) . . ?
Si2 N2 Li1 117.2(3) . . ?
C7 N2 Li2 144.8(3) . . ?
Si2 N2 Li2 100.6(2) . . ?
Li1 N2 Li2 68.5(3) . . ?
C7 N2 Li4 95.5(3) . . ?
Si2 N2 Li4 117.4(3) . . ?
Li1 N2 Li4 116.4(3) . . ?
Li2 N2 Li4 71.9(3) . . ?
C14 N3 Si3 118.2(3) . . ?
C14 N3 Li2 106.1(3) . . ?
Si3 N3 Li2 121.4(3) . . ?
C14 N3 Li4 112.8(3) . . ?
Si3 N3 Li4 115.0(3) . . ?
Li2 N3 Li4 76.1(3) . . ?
C20 N4 Si4 113.8(3) . . ?
C20 N4 Li1 145.2(3) . . ?
Si4 N4 Li1 100.7(3) . . ?
C20 N4 Li2 89.4(3) . . ?
Si4 N4 Li2 119.9(3) . . ?
Li1 N4 Li2 68.7(3) . . ?
C20 N4 Li3 96.2(3) . . ?
Si4 N4 Li3 114.3(3) . . ?
Li1 N4 Li3 72.5(3) . . ?
Li2 N4 Li3 117.2(3) . . ?
N1 C1 C2 120.9(4) . . ?
N1 C1 C6 122.8(3) . . ?
C2 C1 C6 116.2(4) . . ?
C3 C2 C1 123.2(4) . . ?
C3 C2 H2 118.4 . . ?
C1 C2 H2 118.4 . . ?
C2 C3 C4 120.4(4) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 118.4(4) . . ?
C3 C4 H4 120.8 . . ?
C5 C4 H4 120.8 . . ?
C4 C5 C6 122.2(4) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C7 118.5(4) . . ?
C1 C6 C7 121.9(4) . . ?
N2 C7 C6 113.7(3) . . ?
N2 C7 H7B 108.8 . . ?
C6 C7 H7B 108.8 . . ?
N2 C7 H7A 108.8 . . ?
C6 C7 H7A 108.8 . . ?
H7B C7 H7A 107.7 . . ?
Si1 C8 H8C 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8C C8 H8B 109.5 . . ?
Si1 C8 H8A 109.5 . . ?
H8C C8 H8A 109.5 . . ?
H8B C8 H8A 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9C C9 H9B 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
H9C C9 H9A 109.5 . . ?
H9B C9 H9A 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10C C10 H10B 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
H10C C10 H10A 109.5 . . ?
H10B C10 H10A 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11C C11 H11B 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
H11C C11 H11A 109.5 . . ?
H11B C11 H11A 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12C C12 H12B 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
H12C C12 H12A 109.5 . . ?
H12B C12 H12A 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13C C13 H13B 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
H13C C13 H13A 109.5 . . ?
H13B C13 H13A 109.5 . . ?
C15 C14 C19 116.9(4) . . ?
C15 C14 N3 121.4(4) . . ?
C19 C14 N3 121.7(4) . . ?
C16 C15 C14 123.3(4) . . ?
C16 C15 H15 118.4 . . ?
C14 C15 H15 118.4 . . ?
C15 C16 C17 120.1(4) . . ?
C15 C16 H16 119.9 . . ?
C17 C16 H16 119.9 . . ?
C16 C17 C18 118.4(4) . . ?
C16 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
C17 C18 C19 122.3(4) . . ?
C17 C18 H18 118.9 . . ?
C19 C18 H18 118.9 . . ?
C18 C19 C14 118.9(4) . . ?
C18 C19 C20 118.6(4) . . ?
C14 C19 C20 122.5(4) . . ?
N4 C20 C19 113.3(3) . . ?
N4 C20 H20B 108.9 . . ?
C19 C20 H20B 108.9 . . ?
N4 C20 H20A 108.9 . . ?
C19 C20 H20A 108.9 . . ?
H20B C20 H20A 107.7 . . ?
Si3 C21 H21C 109.5 . . ?
Si3 C21 H21B 109.5 . . ?
H21C C21 H21B 109.5 . . ?
Si3 C21 H21A 109.5 . . ?
H21C C21 H21A 109.5 . . ?
H21B C21 H21A 109.5 . . ?
Si3 C22 H22C 109.5 . . ?
Si3 C22 H22B 109.5 . . ?
H22C C22 H22B 109.5 . . ?
Si3 C22 H22A 109.5 . . ?
H22C C22 H22A 109.5 . . ?
H22B C22 H22A 109.5 . . ?
Si3 C23 H23C 109.5 . . ?
Si3 C23 H23B 109.5 . . ?
H23C C23 H23B 109.5 . . ?
Si3 C23 H23A 109.5 . . ?
H23C C23 H23A 109.5 . . ?
H23B C23 H23A 109.5 . . ?
Si4 C24 H24C 109.5 . . ?
Si4 C24 H24B 109.5 . . ?
H24C C24 H24B 109.5 . . ?
Si4 C24 H24A 109.5 . . ?
H24C C24 H24A 109.5 . . ?
H24B C24 H24A 109.5 . . ?
Si4 C25 H25C 109.5 . . ?
Si4 C25 H25B 109.5 . . ?
H25C C25 H25B 109.5 . . ?
Si4 C25 H25A 109.5 . . ?
H25C C25 H25A 109.5 . . ?
H25B C25 H25A 109.5 . . ?
Si4 C26 H26C 109.5 . . ?
Si4 C26 H26B 109.5 . . ?
H26C C26 H26B 109.5 . . ?
Si4 C26 H26A 109.5 . . ?
H26C C26 H26A 109.5 . . ?
H26B C26 H26A 109.5 . . ?
O1 C30 C29 106.6(4) . . ?
O1 C30 H30B 110.4 . . ?
C29 C30 H30B 110.4 . . ?
O1 C30 H30A 110.4 . . ?
C29 C30 H30A 110.4 . . ?
H30B C30 H30A 108.6 . . ?
O2 C31 C32 107.0(4) . . ?
O2 C31 H31B 110.3 . . ?
C32 C31 H31B 110.3 . . ?
O2 C31 H31A 110.3 . . ?
C32 C31 H31A 110.3 . . ?
H31B C31 H31A 108.6 . . ?
C33 C32 C31 103.0(4) . . ?
C33 C32 H32B 111.2 . . ?
C31 C32 H32B 111.2 . . ?
C33 C32 H32A 111.2 . . ?
C31 C32 H32A 111.2 . . ?
H32B C32 H32A 109.1 . . ?
C34 C33 C32 102.9(4) . . ?
C34 C33 H33B 111.2 . . ?
C32 C33 H33B 111.2 . . ?
C34 C33 H33A 111.2 . . ?
C32 C33 H33A 111.2 . . ?
H33B C33 H33A 109.1 . . ?
O2 C34 C33 104.9(4) . . ?
O2 C34 H34B 110.8 . . ?
C33 C34 H34B 110.8 . . ?
O2 C34 H34A 110.8 . . ?
C33 C34 H34A 110.8 . . ?
H34B C34 H34A 108.8 . . ?
N1 Li1 N4 108.8(3) . . ?
N1 Li1 N2 115.0(4) . . ?
N4 Li1 N2 112.0(3) . . ?
N1 Li1 Li2 131.3(4) . . ?
N4 Li1 Li2 55.9(3) . . ?
N2 Li1 Li2 56.2(3) . . ?
N1 Li1 Li3 53.4(2) . . ?
N4 Li1 Li3 55.4(3) . . ?
N2 Li1 Li3 134.7(4) . . ?
Li2 Li1 Li3 96.7(3) . . ?
N3 Li2 N4 114.4(4) . . ?
N3 Li2 N2 107.7(4) . . ?
N4 Li2 N2 110.8(3) . . ?
N3 Li2 Li1 128.7(4) . . ?
N4 Li2 Li1 55.4(3) . . ?
N2 Li2 Li1 55.4(3) . . ?
N3 Li2 Li4 52.9(3) . . ?
N4 Li2 Li4 133.7(4) . . ?
N2 Li2 Li4 54.9(3) . . ?
Li1 Li2 Li4 95.6(4) . . ?
O1 Li3 N1 121.9(4) . . ?
O1 Li3 N4 130.0(4) . . ?
N1 Li3 N4 102.9(3) . . ?
O1 Li3 Li1 158.6(4) . . ?
N1 Li3 Li1 50.9(2) . . ?
N4 Li3 Li1 52.1(2) . . ?
O2 Li4 N3 122.3(4) . . ?
O2 Li4 N2 129.5(4) . . ?
N3 Li4 N2 104.1(3) . . ?
O2 Li4 Li2 158.8(4) . . ?
N3 Li4 Li2 51.0(3) . . ?
N2 Li4 Li2 53.2(3) . . ?
O1 C27 C28 104.1(6) . . ?
O1 C27 H27A 110.9 . . ?
C28 C27 H27A 110.9 . . ?
O1 C27 H27B 110.9 . . ?
C28 C27 H27B 110.9 . . ?
H27A C27 H27B 109 . . ?
C29 C28 C27 103.5(7) . . ?
C29 C28 H28A 111.1 . . ?
C27 C28 H28A 111.1 . . ?
C29 C28 H28B 111.1 . . ?
C27 C28 H28B 111.1 . . ?
H28A C28 H28B 109 . . ?
C28 C29 C30 106.0(5) . . ?
C28 C29 H29A 110.5 . . ?
C30 C29 H29A 110.5 . . ?
C28 C29 H29B 110.5 . . ?
C30 C29 H29B 110.5 . . ?
H29A C29 H29B 108.7 . . ?
H28C C28A H28D 109.1 . . ?
#===END
data_(11b)-oct1696
_database_code_depnum_ccdc_archive 'CCDC 819596'
#TrackingRef '- Combined_cif.cif'
_audit_creation_date 2011-03-17T10:19:30-00:00
_audit_creation_method 'WinGX routine CIF_UPDATE'
_audit_conform_dict_name cif_core.dic
_audit_conform_dict_version 2.2
_audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic
#----------------------------------------------------------------------------#
# CHEMICAL INFORMATION #
#----------------------------------------------------------------------------#
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C34 H64 Mg2 N4 O2 Si4, C7 H8'
_chemical_formula_sum 'C41 H72 Mg2 N4 O2 Si4'
_chemical_formula_weight 814.01
_chemical_compound_source 'synthesis as described'
#----------------------------------------------------------------------------#
# UNIT CELL INFORMATION #
#----------------------------------------------------------------------------#
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
_symmetry_space_group_name_Hall '-P 1'
_symmetry_Int_Tables_number 2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 10.380(5)
_cell_length_b 10.726(3)
_cell_length_c 11.752(4)
_cell_angle_alpha 77.64(2)
_cell_angle_beta 66.68(3)
_cell_angle_gamma 82.20(3)
_cell_volume 1171.8(8)
_cell_formula_units_Z 1
_cell_measurement_temperature 173(2)
_cell_measurement_reflns_used 25
_cell_measurement_theta_min 7
_cell_measurement_theta_max 10
_cell_measurement_wavelength 0.71073
#----------------------------------------------------------------------------#
# CRYSTAL INFORMATION #
#----------------------------------------------------------------------------#
_exptl_crystal_description Block
_exptl_crystal_colour Colourless
_exptl_crystal_size_max 0.4
_exptl_crystal_size_mid 0.4
_exptl_crystal_size_min 0.3
_exptl_crystal_density_diffrn 1.154
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 442
_exptl_special_details
;
?
;
#----------------------------------------------------------------------------#
# ABSORPTION CORRECTION #
#----------------------------------------------------------------------------#
_exptl_absorpt_coefficient_mu 0.19
_exptl_absorpt_correction_type psi-scan
_exptl_absorpt_process_details
;
North A.C.T., Phillips D.C. & Mathews F.S. (1968) Acta. Cryst. A24, 351
Number of psi-scan sets used was 1
Theta correction was applied.
Averaged transmission function was used.
No Fourier smoothing was applied.
;
_exptl_absorpt_correction_T_min 0.95
_exptl_absorpt_correction_T_max 1.00
#----------------------------------------------------------------------------#
# DATA COLLECTION #
#----------------------------------------------------------------------------#
_diffrn_ambient_temperature 173(2)
_diffrn_radiation_wavelength 0.7107
_diffrn_radiation_type MoK\a
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_measurement_device 'Enraf-Nonius CAD4'
_diffrn_measurement_method 'omega-2theta scans'
_diffrn_standards_number ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_av_unetI/netI 0.0512
_diffrn_reflns_number 4120
_diffrn_reflns_limit_h_min 0
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_l_min -12
_diffrn_reflns_limit_l_max 13
_diffrn_reflns_theta_min 2.14
_diffrn_reflns_theta_max 24.98
_diffrn_reflns_theta_full 24.98
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_reflns_number_total 4120
_reflns_number_gt 3392
_reflns_threshold_expression >2sigma(I)
#----------------------------------------------------------------------------#
# COMPUTER PROGRAMS USED #
#----------------------------------------------------------------------------#
_computing_data_collection 'Enraf-Nonius CAD4 software'
_computing_cell_refinement ?
_computing_data_reduction ?
_computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)'
_computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)'
_computing_molecular_graphics ?
_computing_publication_material ?
#----------------------------------------------------------------------------#
# REFINEMENT INFORMATION #
#----------------------------------------------------------------------------#
_refine_special_details
;
There is a molecule of toluene solvate disordered across an inversion centre
for which the H atoms were omitted
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^)+(0.0591P)^2^+0.7873P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens geom
_refine_ls_hydrogen_treatment constr
_refine_ls_extinction_method none
_refine_ls_number_reflns 4120
_refine_ls_number_parameters 253
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0586
_refine_ls_R_factor_gt 0.047
_refine_ls_wR_factor_ref 0.1305
_refine_ls_wR_factor_gt 0.1229
_refine_ls_goodness_of_fit_ref 1.058
_refine_ls_restrained_S_all 1.058
_refine_ls_shift/su_max 0
_refine_ls_shift/su_mean 0
_refine_diff_density_max 0.333
_refine_diff_density_min -0.404
_refine_diff_density_rms 0.083
#----------------------------------------------------------------------------#
# ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS #
#----------------------------------------------------------------------------#
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 0 '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 0.006 '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'
Mg Mg 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mg Mg -0.07704(8) 0.11543(7) -0.03946(7) 0.01657(19) Uani 1 1 d . . .
O O -0.24094(17) 0.21250(15) 0.08495(16) 0.0251(4) Uani 1 1 d . . .
N1 N 0.10880(19) 0.08269(17) -0.00417(17) 0.0176(4) Uani 1 1 d . . .
N2 N -0.0214(2) 0.24764(18) -0.20070(18) 0.0217(4) Uani 1 1 d . . .
Si1 Si 0.13797(7) 0.16647(6) 0.09320(6) 0.02446(19) Uani 1 1 d . . .
Si2 Si -0.13324(7) 0.29307(7) -0.27962(7) 0.0281(2) Uani 1 1 d . . .
C1 C 0.2192(2) 0.2418(2) -0.2093(2) 0.0203(5) Uani 1 1 d . . .
C2 C 0.1061(2) 0.3049(2) -0.2420(2) 0.0216(5) Uani 1 1 d . . .
C3 C 0.1308(3) 0.4271(2) -0.3174(3) 0.0344(6) Uani 1 1 d . . .
H3 H 0.0576 0.4729 -0.3409 0.041 Uiso 1 1 calc R . .
C4 C 0.2582(3) 0.4833(3) -0.3587(3) 0.0391(7) Uani 1 1 d . . .
H4 H 0.271 0.5653 -0.4108 0.047 Uiso 1 1 calc R . .
C5 C 0.3662(3) 0.4210(3) -0.3248(3) 0.0337(6) Uani 1 1 d . . .
H5 H 0.4533 0.4592 -0.3519 0.04 Uiso 1 1 calc R . .
C6 C 0.3439(3) 0.3010(2) -0.2499(2) 0.0272(6) Uani 1 1 d . . .
H6 H 0.4174 0.2576 -0.2254 0.033 Uiso 1 1 calc R . .
C7 C 0.2103(2) 0.1060(2) -0.1386(2) 0.0196(5) Uani 1 1 d . . .
H7A H 0.1854 0.0528 -0.1853 0.024 Uiso 1 1 calc R . .
H7B H 0.3052 0.0749 -0.1401 0.024 Uiso 1 1 calc R . .
C8 C 0.0158(3) 0.1064(3) 0.2567(3) 0.0384(7) Uani 1 1 d . . .
H8A H -0.0809 0.1356 0.2659 0.046 Uiso 1 1 calc R . .
H8B H 0.0403 0.1394 0.3167 0.046 Uiso 1 1 calc R . .
H8C H 0.0237 0.0128 0.2734 0.046 Uiso 1 1 calc R . .
C9 C 0.3264(3) 0.1469(3) 0.0788(3) 0.0421(7) Uani 1 1 d . . .
H9A H 0.3307 0.1521 0.1594 0.051 Uiso 1 1 calc R . .
H9B H 0.3798 0.2148 0.0134 0.051 Uiso 1 1 calc R . .
H9C H 0.3669 0.0635 0.0559 0.051 Uiso 1 1 calc R . .
C10 C 0.1046(3) 0.3437(3) 0.0609(3) 0.0425(7) Uani 1 1 d . . .
H10A H 0.1843 0.3812 -0.0118 0.051 Uiso 1 1 calc R . .
H10B H 0.0931 0.3793 0.1347 0.051 Uiso 1 1 calc R . .
H10C H 0.0188 0.3634 0.0429 0.051 Uiso 1 1 calc R . .
C11 C -0.0473(4) 0.2705(3) -0.4474(3) 0.0489(8) Uani 1 1 d . . .
H11A H -0.1117 0.3031 -0.4909 0.059 Uiso 1 1 calc R . .
H11B H -0.0239 0.1794 -0.4505 0.059 Uiso 1 1 calc R . .
H11C H 0.0388 0.3173 -0.4888 0.059 Uiso 1 1 calc R . .
C12 C -0.2190(3) 0.4601(3) -0.2784(3) 0.0449(8) Uani 1 1 d . . .
H12A H -0.2928 0.4681 -0.3122 0.054 Uiso 1 1 calc R . .
H12B H -0.1483 0.5222 -0.3306 0.054 Uiso 1 1 calc R . .
H12C H -0.2604 0.4766 -0.1919 0.054 Uiso 1 1 calc R . .
C13 C -0.2836(3) 0.1868(3) -0.1976(3) 0.0449(8) Uani 1 1 d . . .
H13A H -0.3459 0.2028 -0.2443 0.054 Uiso 1 1 calc R . .
H13B H -0.3359 0.2044 -0.1122 0.054 Uiso 1 1 calc R . .
H13C H -0.2478 0.0972 -0.1933 0.054 Uiso 1 1 calc R . .
C14 C -0.3739(3) 0.1740(2) 0.1841(3) 0.0319(6) Uani 1 1 d . . .
H14A H -0.3584 0.1216 0.2584 0.038 Uiso 1 1 calc R . .
H14B H -0.4231 0.1232 0.1542 0.038 Uiso 1 1 calc R . .
C15 C -0.4595(3) 0.2966(3) 0.2175(3) 0.0382(7) Uani 1 1 d . . .
H15A H -0.5597 0.2894 0.234 0.046 Uiso 1 1 calc R . .
H15B H -0.4524 0.3183 0.2925 0.046 Uiso 1 1 calc R . .
C16 C -0.3931(3) 0.3949(3) 0.1017(3) 0.0390(7) Uani 1 1 d . . .
H16A H -0.4276 0.3922 0.0349 0.047 Uiso 1 1 calc R . .
H16B H -0.4109 0.4823 0.1216 0.047 Uiso 1 1 calc R . .
C17 C -0.2413(3) 0.3523(2) 0.0646(3) 0.0355(7) Uani 1 1 d . . .
H17A H -0.1875 0.3874 -0.0248 0.043 Uiso 1 1 calc R . .
H17B H -0.2003 0.3797 0.1177 0.043 Uiso 1 1 calc R . .
C1S C 0.5805(9) -0.0195(9) 0.5133(6) 0.062(2) Uani 0.5 1 d P . .
C2S C 0.5181(8) -0.1032(5) 0.4729(4) 0.0801(15) Uani 1 1 d . . .
C3S C 0.4071(13) -0.0967(13) 0.4609(8) 0.087(3) Uani 0.5 1 d P . .
C4S C 0.3031(7) 0.0293(8) 0.4733(5) 0.123(2) Uani 1 1 d . . .
C5S C 0.3702(16) 0.1147(13) 0.5170(8) 0.099(5) Uani 0.5 1 d P . .
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
Mg 0.0160(4) 0.0139(4) 0.0192(4) -0.0009(3) -0.0069(3) -0.0008(3)
O 0.0233(9) 0.0162(8) 0.0294(9) -0.0042(7) -0.0036(7) 0.0001(7)
N1 0.0180(10) 0.0148(9) 0.0201(10) -0.0014(7) -0.0074(8) -0.0032(7)
N2 0.0197(10) 0.0206(10) 0.0221(10) 0.0027(8) -0.0083(8) -0.0014(8)
Si1 0.0277(4) 0.0243(4) 0.0261(4) -0.0056(3) -0.0125(3) -0.0073(3)
Si2 0.0258(4) 0.0297(4) 0.0286(4) 0.0032(3) -0.0153(3) 0.0014(3)
C1 0.0222(12) 0.0189(11) 0.0183(11) -0.0026(9) -0.0063(9) -0.0016(9)
C2 0.0216(12) 0.0204(12) 0.0200(12) -0.0018(9) -0.0055(10) -0.0025(9)
C3 0.0344(15) 0.0256(14) 0.0385(16) 0.0090(12) -0.0155(13) -0.0044(11)
C4 0.0421(17) 0.0254(14) 0.0432(17) 0.0108(12) -0.0142(14) -0.0133(12)
C5 0.0318(15) 0.0325(15) 0.0344(15) 0.0004(12) -0.0091(12) -0.0153(12)
C6 0.0236(13) 0.0292(13) 0.0271(13) -0.0031(10) -0.0079(11) -0.0047(10)
C7 0.0164(11) 0.0191(12) 0.0238(12) -0.0050(9) -0.0079(10) 0.0003(9)
C8 0.0438(17) 0.0466(17) 0.0275(14) -0.0116(12) -0.0112(13) -0.0113(14)
C9 0.0373(16) 0.0499(18) 0.0482(18) -0.0039(14) -0.0240(14) -0.0154(14)
C10 0.0489(18) 0.0284(15) 0.0533(19) -0.0177(13) -0.0156(15) -0.0072(13)
C11 0.058(2) 0.057(2) 0.0322(16) -0.0003(14) -0.0247(15) 0.0038(16)
C12 0.0402(17) 0.0371(16) 0.0504(19) 0.0066(14) -0.0205(15) 0.0088(13)
C13 0.0299(15) 0.0495(19) 0.060(2) 0.0018(15) -0.0270(15) -0.0044(13)
C14 0.0231(13) 0.0248(13) 0.0361(15) -0.0067(11) 0.0014(11) -0.0008(10)
C15 0.0275(14) 0.0289(15) 0.0494(18) -0.0149(13) -0.0031(13) 0.0036(11)
C16 0.0422(17) 0.0228(14) 0.0513(18) -0.0112(13) -0.0186(14) 0.0104(12)
C17 0.0385(16) 0.0187(13) 0.0421(16) -0.0065(11) -0.0074(13) -0.0005(11)
C1S 0.057(5) 0.092(7) 0.018(3) 0.002(4) 0.003(3) -0.012(5)
C2S 0.116(5) 0.071(3) 0.030(2) -0.0183(19) 0.007(3) -0.020(3)
C3S 0.095(8) 0.135(10) 0.034(4) -0.011(5) -0.015(5) -0.052(7)
C4S 0.104(5) 0.177(7) 0.054(3) -0.003(4) 0.007(3) -0.041(5)
C5S 0.117(10) 0.102(8) 0.030(4) -0.009(5) 0.005(6) 0.048(8)
#----------------------------------------------------------------------------#
# MOLECULAR GEOMETRY #
#----------------------------------------------------------------------------#
_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
Mg N2 2.035(2) . ?
Mg O 2.078(2) . ?
Mg N1 2.099(2) . ?
Mg N1 2.116(2) 2 ?
Mg C7 2.735(3) . ?
Mg Mg 2.9438(18) 2 ?
Mg Si2 3.2613(14) . ?
O C14 1.452(3) . ?
O C17 1.467(3) . ?
N1 C7 1.501(3) . ?
N1 Si1 1.731(2) . ?
N1 Mg 2.116(2) 2 ?
N2 C2 1.396(3) . ?
N2 Si2 1.717(2) . ?
Si1 C8 1.865(3) . ?
Si1 C10 1.869(3) . ?
Si1 C9 1.881(3) . ?
Si2 C13 1.867(3) . ?
Si2 C11 1.870(3) . ?
Si2 C12 1.889(3) . ?
C1 C6 1.382(3) . ?
C1 C2 1.419(3) . ?
C1 C7 1.510(3) . ?
C2 C3 1.409(3) . ?
C3 C4 1.389(4) . ?
C3 H3 0.95 . ?
C4 C5 1.378(4) . ?
C4 H4 0.95 . ?
C5 C6 1.385(4) . ?
C5 H5 0.95 . ?
C6 H6 0.95 . ?
C7 H7A 0.99 . ?
C7 H7B 0.99 . ?
C8 H8A 0.98 . ?
C8 H8B 0.98 . ?
C8 H8C 0.98 . ?
C9 H9A 0.98 . ?
C9 H9B 0.98 . ?
C9 H9C 0.98 . ?
C10 H10A 0.98 . ?
C10 H10B 0.98 . ?
C10 H10C 0.98 . ?
C11 H11A 0.98 . ?
C11 H11B 0.98 . ?
C11 H11C 0.98 . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 H13A 0.98 . ?
C13 H13B 0.98 . ?
C13 H13C 0.98 . ?
C14 C15 1.517(4) . ?
C14 H14A 0.99 . ?
C14 H14B 0.99 . ?
C15 C16 1.510(4) . ?
C15 H15A 0.99 . ?
C15 H15B 0.99 . ?
C16 C17 1.492(4) . ?
C16 H16A 0.99 . ?
C16 H16B 0.99 . ?
C17 H17A 0.99 . ?
C17 H17B 0.99 . ?
C1S C5S 1.141(13) 2_656 ?
C1S C4S 1.267(10) 2_656 ?
C1S C3S 1.377(15) 2_656 ?
C1S C2S 1.427(11) . ?
C1S C2S 1.549(11) 2_656 ?
C1S C1S 1.797(18) 2_656 ?
C2S C5S 1.199(14) 2_656 ?
C2S C3S 1.206(11) . ?
C2S C1S 1.549(11) 2_656 ?
C3S C1S 1.377(15) 2_656 ?
C3S C4S 1.605(15) . ?
C4S C1S 1.267(10) 2_656 ?
C4S C5S 1.498(18) . ?
C5S C1S 1.141(13) 2_656 ?
C5S C2S 1.199(14) 2_656 ?
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 Mg O 102.15(8) . . ?
N2 Mg N1 102.31(9) . . ?
O Mg N1 115.36(8) . . ?
N2 Mg N1 134.60(9) . 2 ?
O Mg N1 110.57(8) . 2 ?
N1 Mg N1 91.39(8) . 2 ?
N2 Mg C7 73.99(8) . . ?
O Mg C7 137.91(8) . . ?
N1 Mg C7 32.95(7) . . ?
N1 Mg C7 99.40(8) 2 . ?
N2 Mg Mg 131.05(7) . 2 ?
O Mg Mg 123.91(7) . 2 ?
N1 Mg Mg 45.94(6) . 2 ?
N1 Mg Mg 45.45(6) 2 2 ?
C7 Mg Mg 61.26(6) . 2 ?
N2 Mg Si2 26.99(6) . . ?
O Mg Si2 91.20(6) . . ?
N1 Mg Si2 129.01(6) . . ?
N1 Mg Si2 120.27(6) 2 . ?
C7 Mg Si2 98.67(6) . . ?
Mg Mg Si2 144.20(4) 2 . ?
C14 O C17 107.75(18) . . ?
C14 O Mg 133.28(14) . . ?
C17 O Mg 118.33(15) . . ?
C7 N1 Si1 114.54(14) . . ?
C7 N1 Mg 97.54(13) . . ?
Si1 N1 Mg 121.19(10) . . ?
C7 N1 Mg 105.30(14) . 2 ?
Si1 N1 Mg 124.22(10) . 2 ?
Mg N1 Mg 88.61(8) . 2 ?
C2 N2 Si2 120.90(16) . . ?
C2 N2 Mg 118.53(16) . . ?
Si2 N2 Mg 120.49(11) . . ?
N1 Si1 C8 106.60(11) . . ?
N1 Si1 C10 115.53(12) . . ?
C8 Si1 C10 107.52(14) . . ?
N1 Si1 C9 112.01(13) . . ?
C8 Si1 C9 111.68(14) . . ?
C10 Si1 C9 103.51(15) . . ?
N2 Si2 C13 106.21(12) . . ?
N2 Si2 C11 111.81(13) . . ?
C13 Si2 C11 108.60(16) . . ?
N2 Si2 C12 117.90(13) . . ?
C13 Si2 C12 104.18(15) . . ?
C11 Si2 C12 107.56(15) . . ?
N2 Si2 Mg 32.53(7) . . ?
C13 Si2 Mg 73.87(10) . . ?
C11 Si2 Mg 126.58(11) . . ?
C12 Si2 Mg 123.90(11) . . ?
C6 C1 C2 120.2(2) . . ?
C6 C1 C7 118.6(2) . . ?
C2 C1 C7 121.1(2) . . ?
N2 C2 C3 122.8(2) . . ?
N2 C2 C1 121.2(2) . . ?
C3 C2 C1 116.0(2) . . ?
C4 C3 C2 122.5(3) . . ?
C4 C3 H3 118.7 . . ?
C2 C3 H3 118.7 . . ?
C5 C4 C3 120.5(2) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
C4 C5 C6 117.9(2) . . ?
C4 C5 H5 121 . . ?
C6 C5 H5 121 . . ?
C1 C6 C5 122.8(2) . . ?
C1 C6 H6 118.6 . . ?
C5 C6 H6 118.6 . . ?
N1 C7 C1 117.46(19) . . ?
N1 C7 Mg 49.51(10) . . ?
C1 C7 Mg 94.37(14) . . ?
N1 C7 H7A 107.9 . . ?
C1 C7 H7A 107.9 . . ?
Mg C7 H7A 75.5 . . ?
N1 C7 H7B 107.9 . . ?
C1 C7 H7B 107.9 . . ?
Mg C7 H7B 154.9 . . ?
H7A C7 H7B 107.2 . . ?
Si1 C8 H8A 109.5 . . ?
Si1 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
Si1 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
Si1 C9 H9A 109.5 . . ?
Si1 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
Si1 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
Si1 C10 H10A 109.5 . . ?
Si1 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
Si1 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Si2 C11 H11A 109.5 . . ?
Si2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
Si2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
Si2 C12 H12A 109.5 . . ?
Si2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
Si2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
Si2 C13 H13A 109.5 . . ?
Si2 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
Si2 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O C14 C15 106.2(2) . . ?
O C14 H14A 110.5 . . ?
C15 C14 H14A 110.5 . . ?
O C14 H14B 110.5 . . ?
C15 C14 H14B 110.5 . . ?
H14A C14 H14B 108.7 . . ?
C16 C15 C14 103.3(2) . . ?
C16 C15 H15A 111.1 . . ?
C14 C15 H15A 111.1 . . ?
C16 C15 H15B 111.1 . . ?
C14 C15 H15B 111.1 . . ?
H15A C15 H15B 109.1 . . ?
C17 C16 C15 101.5(2) . . ?
C17 C16 H16A 111.5 . . ?
C15 C16 H16A 111.5 . . ?
C17 C16 H16B 111.5 . . ?
C15 C16 H16B 111.5 . . ?
H16A C16 H16B 109.3 . . ?
O C17 C16 104.0(2) . . ?
O C17 H17A 111 . . ?
C16 C17 H17A 111 . . ?
O C17 H17B 111 . . ?
C16 C17 H17B 111 . . ?
H17A C17 H17B 109 . . ?
C5S C1S C4S 76.8(11) 2_656 2_656 ?
C5S C1S C3S 150.2(13) 2_656 2_656 ?
C4S C1S C3S 74.6(9) 2_656 2_656 ?
C5S C1S C2S 54.3(9) 2_656 . ?
C4S C1S C2S 131.0(10) 2_656 . ?
C3S C1S C2S 153.5(10) 2_656 . ?
C5S C1S C2S 159.1(12) 2_656 2_656 ?
C4S C1S C2S 122.9(9) 2_656 2_656 ?
C3S C1S C2S 48.2(6) 2_656 2_656 ?
C2S C1S C2S 105.8(6) . 2_656 ?
C5S C1S C1S 110.0(13) 2_656 2_656 ?
C4S C1S C1S 171.5(12) 2_656 2_656 ?
C3S C1S C1S 97.9(10) 2_656 2_656 ?
C2S C1S C1S 56.0(6) . 2_656 ?
C2S C1S C1S 49.8(5) 2_656 2_656 ?
C5S C2S C3S 177.2(10) 2_656 . ?
C5S C2S C1S 50.6(7) 2_656 . ?
C3S C2S C1S 132.2(8) . . ?
C5S C2S C1S 124.4(9) 2_656 2_656 ?
C3S C2S C1S 58.4(7) . 2_656 ?
C1S C2S C1S 74.2(6) . 2_656 ?
C2S C3S C1S 73.3(7) . 2_656 ?
C2S C3S C4S 122.9(9) . . ?
C1S C3S C4S 49.5(6) 2_656 . ?
C1S C4S C5S 47.8(6) 2_656 . ?
C1S C4S C3S 55.8(7) 2_656 . ?
C5S C4S C3S 103.3(8) . . ?
C1S C5S C2S 75.1(9) 2_656 2_656 ?
C1S C5S C4S 55.4(9) 2_656 . ?
C2S C5S C4S 130.5(10) 2_656 . ?
#===END