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#$Date: 2025-08-22 00:26:11 +0300 (Fri, 22 Aug 2025) $
#$Revision: 301853 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/86/7108651.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7108651
loop_
_publ_author_name
'Zhu, Xiancui'
'Zhou, Shuangliu'
'Wang, Shaowu'
'Wei, Yun'
'Zhang, Lijun'
'Wang, Fenhua'
'Wang, Shaoyin'
'Feng, Zhijun'
_publ_section_title
;
 Rare-earth metal complexes having an unusual indolyl-1,2-dianion through
 C--H activation with a novel \h1:(\m2--\h1:\h1) bonding with metals
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   98
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              12020
_journal_page_last               12022
_journal_paper_doi               10.1039/c2cc36045d
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C38 H66 Li4 N6 Si4'
_chemical_formula_weight         747.09
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                97.2570(10)
_cell_angle_beta                 100.0590(10)
_cell_angle_gamma                101.9070(10)
_cell_formula_units_Z            1
_cell_length_a                   9.1116(8)
_cell_length_b                   11.2374(10)
_cell_length_c                   12.0801(11)
_cell_measurement_reflns_used    4019
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.04
_cell_measurement_theta_min      2.33
_cell_volume                     1174.63(18)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0211
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9138
_diffrn_reflns_theta_full        25.99
_diffrn_reflns_theta_max         25.99
_diffrn_reflns_theta_min         1.74
_exptl_absorpt_coefficient_mu    0.157
_exptl_absorpt_correction_T_max  0.9633
_exptl_absorpt_correction_T_min  0.9529
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.056
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.195
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         4549
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0434
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0677P)²+0.2602P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1204
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                3447
_reflns_number_total             4549
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc36045d.txt
_cod_data_source_block           110307a_0m
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               7108651
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.4054(3) 0.82381(19) 1.06495(17) 0.0495(5) Uani 1 1 d .
Li1 Li 0.2550(5) 0.6666(3) 0.7933(3) 0.0604(9) Uani 1 1 d .
N1 N 0.5463(2) 0.88557(15) 1.04948(15) 0.0555(5) Uani 1 1 d .
Si1 Si 0.32124(6) 0.84548(5) 0.62872(5) 0.04472(17) Uani 1 1 d .
C2 C 0.3137(3) 0.8647(2) 1.1353(2) 0.0644(6) Uani 1 1 d .
H2 H 0.3421 0.9444 1.1768 0.077 Uiso 1 1 calc R
N2 N 0.3616(2) 0.52715(15) 0.79285(15) 0.0531(5) Uani 1 1 d .
Si2 Si 0.05162(6) 0.82895(6) 0.74175(5) 0.04915(18) Uani 1 1 d .
C3 C 0.1816(3) 0.7858(3) 1.1421(2) 0.0818(8) Uani 1 1 d .
H3 H 0.1197 0.8120 1.1891 0.098 Uiso 1 1 calc R
N3 N 0.23650(17) 0.82268(14) 0.74203(13) 0.0393(4) Uani 1 1 d .
C4 C 0.1376(3) 0.6665(3) 1.0798(3) 0.0902(10) Uani 1 1 d .
H4 H 0.0471 0.6143 1.0865 0.108 Uiso 1 1 calc R
C5 C 0.2248(3) 0.6244(2) 1.0089(2) 0.0738(7) Uani 1 1 d .
H5 H 0.1938 0.5447 0.9674 0.089 Uiso 1 1 calc R
C6 C 0.3615(3) 0.70310(19) 0.99990(17) 0.0520(5) Uani 1 1 d .
C7 C 0.4841(3) 0.69046(18) 0.94343(17) 0.0499(5) Uani 1 1 d .
C8 C 0.5910(3) 0.80306(19) 0.97864(18) 0.0538(5) Uani 1 1 d .
H8 H 0.6843 0.8200 0.9557 0.065 Uiso 1 1 calc R
C9 C 0.4864(3) 0.58738(19) 0.85929(18) 0.0546(5) Uani 1 1 d .
H9 H 0.5781 0.5653 0.8538 0.066 Uiso 1 1 calc R
C10 C 0.3521(3) 0.41523(19) 0.70986(19) 0.0596(6) Uani 1 1 d .
C11 C 0.2745(4) 0.4373(3) 0.5954(2) 0.1003(11) Uani 1 1 d .
H11A H 0.1748 0.4507 0.5999 0.150 Uiso 1 1 calc R
H11B H 0.2642 0.3667 0.5384 0.150 Uiso 1 1 calc R
H11C H 0.3352 0.5087 0.5752 0.150 Uiso 1 1 calc R
C12 C 0.2483(4) 0.3105(2) 0.7480(3) 0.0929(10) Uani 1 1 d .
H12A H 0.2975 0.2971 0.8209 0.139 Uiso 1 1 calc R
H12B H 0.2290 0.2365 0.6931 0.139 Uiso 1 1 calc R
H12C H 0.1530 0.3319 0.7542 0.139 Uiso 1 1 calc R
C13 C 0.5054(4) 0.3848(3) 0.7026(3) 0.0915(9) Uani 1 1 d .
H13A H 0.5708 0.4526 0.6811 0.137 Uiso 1 1 calc R
H13B H 0.4895 0.3122 0.6466 0.137 Uiso 1 1 calc R
H13C H 0.5527 0.3702 0.7756 0.137 Uiso 1 1 calc R
C14 C 0.5109(3) 0.8023(2) 0.6518(2) 0.0594(6) Uani 1 1 d .
H14A H 0.5751 0.8504 0.7213 0.089 Uiso 1 1 calc R
H14B H 0.5594 0.8182 0.5890 0.089 Uiso 1 1 calc R
H14C H 0.4954 0.7162 0.6571 0.089 Uiso 1 1 calc R
C15 C 0.3588(3) 1.0109(2) 0.6087(2) 0.0697(7) Uani 1 1 d .
H15A H 0.2633 1.0317 0.5817 0.105 Uiso 1 1 calc R
H15B H 0.4229 1.0229 0.5539 0.105 Uiso 1 1 calc R
H15C H 0.4093 1.0629 0.6801 0.105 Uiso 1 1 calc R
C16 C 0.2096(3) 0.7509(3) 0.4888(2) 0.0760(8) Uani 1 1 d .
H16A H 0.1765 0.6666 0.4982 0.114 Uiso 1 1 calc R
H16B H 0.2735 0.7551 0.4333 0.114 Uiso 1 1 calc R
H16C H 0.1218 0.7826 0.4632 0.114 Uiso 1 1 calc R
C17 C -0.0454(3) 0.8986(3) 0.6261(2) 0.0801(8) Uani 1 1 d .
H17A H 0.0103 0.9820 0.6302 0.120 Uiso 1 1 calc R
H17B H -0.1481 0.8982 0.6351 0.120 Uiso 1 1 calc R
H17C H -0.0483 0.8515 0.5533 0.120 Uiso 1 1 calc R
C18 C -0.0705(3) 0.6710(3) 0.7345(3) 0.0987(11) Uani 1 1 d .
H18A H -0.0586 0.6168 0.6703 0.148 Uiso 1 1 calc R
H18B H -0.1760 0.6751 0.7261 0.148 Uiso 1 1 calc R
H18C H -0.0395 0.6402 0.8033 0.148 Uiso 1 1 calc R
C19 C 0.0416(3) 0.9241(4) 0.8772(3) 0.0996(11) Uani 1 1 d .
H19A H 0.0775 0.8867 0.9406 0.149 Uiso 1 1 calc R
H19B H -0.0626 0.9289 0.8762 0.149 Uiso 1 1 calc R
H19C H 0.1046 1.0056 0.8845 0.149 Uiso 1 1 calc R
Li2 Li 0.6429(5) 1.0613(3) 1.1137(3) 0.0616(10) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Li Li -0.0003 0.0001 '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'
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
N1 C1 C2 128.37(19) . .
N1 C1 C6 110.63(19) . .
C2 C1 C6 121.0(2) . .
N1 C1 Li2 71.94(15) . 2_677
C2 C1 Li2 103.54(18) . 2_677
C6 C1 Li2 95.28(15) . 2_677
N3 Li1 N2 147.8(2) . .
N3 Li1 C7 112.59(18) . .
N2 Li1 C7 62.57(13) . .
N3 Li1 C6 110.20(17) . .
N2 Li1 C6 83.14(16) . .
C7 Li1 C6 33.74(9) . .
N3 Li1 C9 130.8(2) . .
N2 Li1 C9 30.42(9) . .
C7 Li1 C9 33.95(9) . .
C6 Li1 C9 62.35(12) . .
N3 Li1 Li2 41.81(12) . 2_677
N2 Li1 Li2 133.6(2) . 2_677
C7 Li1 Li2 74.41(14) . 2_677
C6 Li1 Li2 69.05(13) . 2_677
C9 Li1 Li2 103.44(16) . 2_677
C8 N1 C1 104.99(17) . .
C8 N1 Li2 130.7(2) . .
C1 N1 Li2 124.14(19) . .
C8 N1 Li2 93.79(15) . 2_677
C1 N1 Li2 77.64(15) . 2_677
Li2 N1 Li2 93.37(15) . 2_677
N3 Si1 C15 112.07(10) . .
N3 Si1 C14 110.05(9) . .
C15 Si1 C14 107.08(11) . .
N3 Si1 C16 114.65(11) . .
C15 Si1 C16 106.97(13) . .
C14 Si1 C16 105.56(12) . .
N3 Si1 Li2 37.56(9) . 2_677
C15 Si1 Li2 87.68(11) . 2_677
C14 Si1 Li2 92.14(11) . 2_677
C16 Si1 Li2 151.99(12) . 2_677
C3 C2 C1 118.7(2) . .
C3 C2 H2 120.7 . .
C1 C2 H2 120.7 . .
C9 N2 C10 122.8(2) . .
C9 N2 Li1 96.65(18) . .
C10 N2 Li1 134.52(18) . .
N3 Si2 C19 109.62(11) . .
N3 Si2 C17 116.90(11) . .
C19 Si2 C17 105.03(15) . .
N3 Si2 C18 110.64(12) . .
C19 Si2 C18 107.18(17) . .
C17 Si2 C18 106.93(15) . .
N3 Si2 Li2 41.97(9) . 2_677
C19 Si2 Li2 67.83(12) . 2_677
C17 Si2 Li2 125.23(13) . 2_677
C18 Si2 Li2 127.43(13) . 2_677
C2 C3 C4 121.1(3) . .
C2 C3 H3 119.4 . .
C4 C3 H3 119.4 . .
Si2 N3 Si1 123.24(9) . .
Si2 N3 Li1 104.69(15) . .
Si1 N3 Li1 112.16(14) . .
Si2 N3 Li2 103.93(14) . 2_677
Si1 N3 Li2 111.58(14) . 2_677
Li1 N3 Li2 98.03(18) . 2_677
C5 C4 C3 121.4(3) . .
C5 C4 H4 119.3 . .
C3 C4 H4 119.3 . .
C4 C5 C6 119.0(2) . .
C4 C5 H5 120.5 . .
C6 C5 H5 120.5 . .
C5 C6 C1 118.8(2) . .
C5 C6 C7 135.0(2) . .
C1 C6 C7 105.96(18) . .
C5 C6 Li1 86.36(17) . .
C1 C6 Li1 121.45(17) . .
C7 C6 Li1 72.91(15) . .
C8 C7 C6 104.70(18) . .
C8 C7 C9 128.4(2) . .
C6 C7 C9 126.57(19) . .
C8 C7 Li1 121.26(17) . .
C6 C7 Li1 73.36(16) . .
C9 C7 Li1 74.54(15) . .
N1 C8 C7 113.7(2) . .
N1 C8 H8 123.2 . .
C7 C8 H8 123.2 . .
N2 C9 C7 119.4(2) . .
N2 C9 Li1 52.93(14) . .
C7 C9 Li1 71.51(15) . .
N2 C9 H9 120.3 . .
C7 C9 H9 120.3 . .
Li1 C9 H9 155.7 . .
N2 C10 C11 106.09(19) . .
N2 C10 C13 114.66(19) . .
C11 C10 C13 110.5(3) . .
N2 C10 C12 105.3(2) . .
C11 C10 C12 109.6(2) . .
C13 C10 C12 110.4(2) . .
C10 C11 H11A 109.5 . .
C10 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C10 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C10 C12 H12A 109.5 . .
C10 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C10 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
Si1 C14 H14A 109.5 . .
Si1 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
Si1 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
Si1 C15 H15A 109.5 . .
Si1 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
Si1 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
Si1 C16 H16A 109.5 . .
Si1 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
Si1 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
Si2 C17 H17A 109.5 . .
Si2 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
Si2 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
Si2 C18 H18A 109.5 . .
Si2 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
Si2 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
Si2 C19 H19A 109.5 . .
Si2 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
Si2 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
N1 Li2 N3 143.4(2) . 2_677
N1 Li2 N1 86.63(15) . 2_677
N3 Li2 N1 126.42(19) 2_677 2_677
N1 Li2 C1 103.51(16) . 2_677
N3 Li2 C1 113.03(17) 2_677 2_677
N1 Li2 C1 30.42(8) 2_677 2_677
N1 Li2 Si2 129.1(2) . 2_677
N3 Li2 Si2 34.10(8) 2_677 2_677
N1 Li2 Si2 138.77(15) 2_677 2_677
C1 Li2 Si2 110.86(14) 2_677 2_677
N1 Li2 Li1 172.1(2) . 2_677
N3 Li2 Li1 40.16(11) 2_677 2_677
N1 Li2 Li1 87.70(14) 2_677 2_677
C1 Li2 Li1 73.90(13) 2_677 2_677
Si2 Li2 Li1 58.35(10) 2_677 2_677
N1 Li2 Si1 119.76(17) . 2_677
N3 Li2 Si1 30.86(7) 2_677 2_677
N1 Li2 Si1 125.48(16) 2_677 2_677
C1 Li2 Si1 130.47(14) 2_677 2_677
Si2 Li2 Si1 59.48(7) 2_677 2_677
Li1 Li2 Si1 59.87(10) 2_677 2_677
N1 Li2 Li2 50.52(11) . 2_677
N3 Li2 Li2 158.9(3) 2_677 2_677
N1 Li2 Li2 36.11(10) 2_677 2_677
C1 Li2 Li2 58.07(13) 2_677 2_677
Si2 Li2 Li2 162.5(2) 2_677 2_677
Li1 Li2 Li2 123.6(2) 2_677 2_677
Si1 Li2 Li2 137.9(2) 2_677 2_677
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.383(3) .
C1 C2 1.393(3) .
C1 C6 1.419(3) .
C1 Li2 2.669(5) 2_677
Li1 N3 1.962(4) .
Li1 N2 2.007(4) .
Li1 C7 2.458(5) .
Li1 C6 2.464(4) .
Li1 C9 2.498(5) .
Li1 Li2 3.012(5) 2_677
N1 C8 1.355(3) .
N1 Li2 1.983(4) .
N1 Li2 2.598(5) 2_677
Si1 N3 1.7063(16) .
Si1 C15 1.874(2) .
Si1 C14 1.874(2) .
Si1 C16 1.877(2) .
Si1 Li2 3.093(4) 2_677
C2 C3 1.361(4) .
C2 H2 0.9300 .
N2 C9 1.273(3) .
N2 C10 1.484(3) .
Si2 N3 1.7000(16) .
Si2 C19 1.865(3) .
Si2 C17 1.865(3) .
Si2 C18 1.873(3) .
Si2 Li2 2.943(4) 2_677
C3 C4 1.394(4) .
C3 H3 0.9300 .
N3 Li2 2.028(4) 2_677
C4 C5 1.371(4) .
C4 H4 0.9300 .
C5 C6 1.401(3) .
C5 H5 0.9300 .
C6 C7 1.428(3) .
C7 C8 1.393(3) .
C7 C9 1.448(3) .
C8 H8 0.9300 .
C9 H9 0.9300 .
C10 C11 1.514(4) .
C10 C13 1.519(4) .
C10 C12 1.524(4) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
Li2 N3 2.028(4) 2_677
Li2 N1 2.598(5) 2_677
Li2 C1 2.669(5) 2_677
Li2 Si2 2.943(4) 2_677
Li2 Li1 3.012(5) 2_677
Li2 Si1 3.093(4) 2_677
Li2 Li2 3.360(8) 2_677
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139182901
