#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:20:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179408 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/05/4330582.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_4330582
loop_
_publ_author_name
'Weiyin Yi'
'Jie Zhang'
'Zhenxia Chen'
'Xigeng Zhou'
_publ_section_title
;
 Me-Si Bond Cleavage of Anionic Bis(trimethylsilyl)amide in
 Scorpionate-Anchored Rare Earth Metal Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10631
_journal_page_last               10638
_journal_paper_doi               10.1021/ic3008552
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C29 H57 B Er N9 Si2'
_chemical_formula_weight         766.09
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.8400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.7039(12)
_cell_length_b                   14.0727(14)
_cell_length_c                   12.2051(12)
_cell_measurement_reflns_used    8145
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      2.30
_cell_volume                     1878.7(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0256
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7715
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    2.328
_exptl_absorpt_correction_T_max  0.8005
_exptl_absorpt_correction_T_min  0.7215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.354
_exptl_crystal_description       prism
_exptl_crystal_F_000             790
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.917
_refine_diff_density_min         -1.271
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3455
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0388
_refine_ls_R_factor_gt           0.0374
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0227P)²+13.3530P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                3317
_reflns_number_total             3455
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008552_si_001_1.cif
_cod_data_source_block           0713ywy
_cod_database_code               4330582
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, 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
Er1 Er 0.18906(3) 0.2500 0.17751(3) 0.02764(13) Uani 1 2 d S
B1 B 0.1969(9) 0.2500 -0.1064(8) 0.037(2) Uani 1 2 d S
Si1 Si 0.5167(2) 0.2500 0.3122(3) 0.0547(7) Uani 1 2 d S
Si2 Si 0.3804(3) 0.2500 0.4699(3) 0.111(2) Uani 1 2 d S
N1 N 0.0497(5) 0.3296(5) 0.2403(5) 0.0647(19) Uani 1 1 d .
N2 N 0.0604(6) 0.2500 -0.1235(6) 0.0404(17) Uani 1 2 d S
N3 N 0.0209(6) 0.2500 -0.0301(6) 0.0372(16) Uani 1 2 d S
N4 N 0.2568(4) 0.1586(4) -0.0430(4) 0.0378(11) Uani 1 1 d .
N5 N 0.2557(4) 0.1345(4) 0.0665(4) 0.0366(11) Uani 1 1 d .
N6 N 0.3747(6) 0.2500 0.3272(6) 0.0440(18) Uani 1 2 d S
C1 C 0.0008(10) 0.2500 0.2620(9) 0.075(4) Uani 1 2 d S
C2 C -0.1045(14) 0.2500 0.3086(14) 0.155(10) Uani 1 2 d S
H2A H -0.1219 0.1859 0.3246 0.233 Uiso 0.50 1 calc PR
H2B H -0.1758 0.2774 0.2511 0.233 Uiso 0.50 1 calc PR
H2C H -0.0817 0.2867 0.3795 0.233 Uiso 0.50 1 calc PR
C3 C -0.0054(11) 0.4270(11) 0.2419(12) 0.143(7) Uani 1 1 d .
H3 H -0.0917 0.4162 0.2300 0.171 Uiso 1 1 calc R
C4 C 0.0506(17) 0.4699(14) 0.3612(16) 0.205(8) Uani 1 1 d U
H4A H 0.0446 0.4259 0.4190 0.307 Uiso 1 1 calc R
H4B H 0.0081 0.5274 0.3650 0.307 Uiso 1 1 calc R
H4C H 0.1351 0.4840 0.3761 0.307 Uiso 1 1 calc R
C5 C -0.0038(12) 0.4816(10) 0.1401(14) 0.138(5) Uani 1 1 d U
H5A H 0.0784 0.4854 0.1411 0.207 Uiso 1 1 calc R
H5B H -0.0343 0.5445 0.1432 0.207 Uiso 1 1 calc R
H5C H -0.0546 0.4507 0.0694 0.207 Uiso 1 1 calc R
C6 C -0.0258(13) 0.2500 -0.3437(10) 0.098(5) Uani 1 2 d S
H6A H -0.0227 0.3143 -0.3688 0.147 Uiso 0.50 1 calc PR
H6B H -0.0955 0.2184 -0.3985 0.147 Uiso 0.50 1 calc PR
H6C H 0.0475 0.2173 -0.3401 0.147 Uiso 0.50 1 calc PR
C7 C -0.0360(9) 0.2500 -0.2255(8) 0.054(3) Uani 1 2 d S
C8 C -0.1392(9) 0.2500 -0.1967(9) 0.061(3) Uani 1 2 d S
H8 H -0.2199 0.2500 -0.2484 0.073 Uiso 1 2 calc SR
C9 C -0.0999(8) 0.2500 -0.0770(8) 0.043(2) Uani 1 2 d S
C10 C -0.1822(9) 0.2500 -0.0056(10) 0.066(3) Uani 1 2 d S
H10A H -0.1987 0.1857 0.0105 0.099 Uiso 0.50 1 calc PR
H10B H -0.2577 0.2814 -0.0489 0.099 Uiso 0.50 1 calc PR
H10C H -0.1426 0.2830 0.0669 0.099 Uiso 0.50 1 calc PR
C11 C 0.3279(9) 0.0904(7) -0.1976(7) 0.087(3) Uani 1 1 d .
H11A H 0.2954 0.1486 -0.2373 0.130 Uiso 1 1 calc R
H11B H 0.2859 0.0375 -0.2444 0.130 Uiso 1 1 calc R
H11C H 0.4135 0.0864 -0.1852 0.130 Uiso 1 1 calc R
C12 C 0.3107(7) 0.0881(5) -0.0815(6) 0.0527(17) Uani 1 1 d .
C13 C 0.3443(7) 0.0179(5) 0.0016(7) 0.063(2) Uani 1 1 d .
H13 H 0.3825 -0.0393 -0.0023 0.075 Uiso 1 1 calc R
C14 C 0.3097(6) 0.0496(5) 0.0929(6) 0.0491(16) Uani 1 1 d .
C15 C 0.3275(8) 0.0002(6) 0.2070(7) 0.068(2) Uani 1 1 d .
H15A H 0.2945 0.0387 0.2535 0.102 Uiso 1 1 calc R
H15B H 0.4132 -0.0098 0.2487 0.102 Uiso 1 1 calc R
H15C H 0.2862 -0.0600 0.1916 0.102 Uiso 1 1 calc R
C16 C 0.5166(10) 0.2500 0.1598(11) 0.109(7) Uani 1 2 d S
H16A H 0.4688 0.1975 0.1173 0.163 Uiso 0.50 1 calc PR
H16B H 0.5990 0.2440 0.1616 0.163 Uiso 0.50 1 calc PR
H16C H 0.4821 0.3084 0.1218 0.163 Uiso 0.50 1 calc PR
C17 C 0.6136(8) 0.3562(8) 0.3801(10) 0.093(3) Uani 1 1 d .
H17A H 0.6190 0.3625 0.4601 0.140 Uiso 1 1 calc R
H17B H 0.5772 0.4124 0.3373 0.140 Uiso 1 1 calc R
H17C H 0.6940 0.3479 0.3776 0.140 Uiso 1 1 calc R
C18 C 0.2515(16) 0.2500 0.5053(15) 0.121(6) Uani 1 2 d SU
H18A H 0.2187 0.3132 0.4976 0.182 Uiso 0.50 1 calc PR
H18B H 0.2715 0.2287 0.5846 0.182 Uiso 0.50 1 calc PR
H18C H 0.1918 0.2081 0.4534 0.182 Uiso 0.50 1 calc PR
C19 C 0.381(2) 0.0991(15) 0.5103(17) 0.094(6) Uani 0.50 1 d PU
H19A H 0.3104 0.0693 0.4553 0.141 Uiso 0.50 1 calc PR
H19B H 0.3807 0.0914 0.5882 0.141 Uiso 0.50 1 calc PR
H19C H 0.4537 0.0702 0.5053 0.141 Uiso 0.50 1 calc PR
C20 C 0.5178(17) 0.2500 0.5921(16) 0.135(7) Uani 1 2 d SU
H20A H 0.5507 0.3132 0.6054 0.203 Uiso 0.50 1 calc PR
H20B H 0.5756 0.2081 0.5775 0.203 Uiso 0.50 1 calc PR
H20C H 0.5020 0.2286 0.6601 0.203 Uiso 0.50 1 calc PR
H1 H 0.208(7) 0.2500 -0.199(7) 0.04(2) Uiso 1 2 d S
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'
B B 0.0013 0.0007 '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'
Er Er -0.2586 4.9576 '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
N6 Er1 N1 108.4(2) . 4_565
N6 Er1 N1 108.4(2) . .
N1 Er1 N1 57.7(4) 4_565 .
N6 Er1 N5 92.49(18) . 4_565
N1 Er1 N5 156.1(2) 4_565 4_565
N1 Er1 N5 105.4(2) . 4_565
N6 Er1 N5 92.49(18) . .
N1 Er1 N5 105.4(2) 4_565 .
N1 Er1 N5 156.1(2) . .
N5 Er1 N5 84.6(2) 4_565 .
N6 Er1 N3 162.5(2) . .
N1 Er1 N3 86.81(19) 4_565 .
N1 Er1 N3 86.81(19) . .
N5 Er1 N3 74.74(16) 4_565 .
N5 Er1 N3 74.74(16) . .
N6 Er1 C1 111.2(3) . .
N1 Er1 C1 28.9(2) 4_565 .
N1 Er1 C1 28.9(2) . .
N5 Er1 C1 132.29(15) 4_565 .
N5 Er1 C1 132.29(15) . .
N3 Er1 C1 86.3(3) . .
N2 B1 N4 109.6(4) . 4_565
N2 B1 N4 109.6(4) . .
N4 B1 N4 113.8(7) 4_565 .
N2 B1 H1 110(4) . .
N4 B1 H1 107(2) 4_565 .
N4 B1 H1 107(2) . .
N6 Si1 C16 116.5(4) . .
N6 Si1 C17 113.8(3) . 4_565
C16 Si1 C17 103.1(4) . 4_565
N6 Si1 C17 113.8(3) . .
C16 Si1 C17 103.1(4) . .
C17 Si1 C17 105.2(7) 4_565 .
C18 Si2 N6 122.4(7) . .
C18 Si2 C20 114.1(9) . .
N6 Si2 C20 123.6(7) . .
C18 Si2 C19 82.9(6) . 4_565
N6 Si2 C19 103.0(5) . 4_565
C20 Si2 C19 83.0(6) . 4_565
C18 Si2 C19 82.9(6) . .
N6 Si2 C19 103.0(5) . .
C20 Si2 C19 83.0(6) . .
C19 Si2 C19 154.0(10) 4_565 .
C1 N1 C3 122.9(8) . .
C1 N1 Er1 93.6(5) . .
C3 N1 Er1 142.4(8) . .
C7 N2 N3 110.3(7) . .
C7 N2 B1 127.8(8) . .
N3 N2 B1 121.9(6) . .
C9 N3 N2 105.3(7) . .
C9 N3 Er1 138.1(6) . .
N2 N3 Er1 116.6(5) . .
C12 N4 N5 108.9(5) . .
C12 N4 B1 128.9(6) . .
N5 N4 B1 122.2(5) . .
C14 N5 N4 106.6(5) . .
C14 N5 Er1 133.3(4) . .
N4 N5 Er1 119.5(4) . .
Si2 N6 Si1 114.4(4) . .
Si2 N6 Er1 119.5(4) . .
Si1 N6 Er1 126.1(4) . .
N1 C1 N1 115.2(9) . 4_565
N1 C1 C2 122.4(4) . .
N1 C1 C2 122.4(4) 4_565 .
N1 C1 Er1 57.6(4) . .
N1 C1 Er1 57.6(4) 4_565 .
C2 C1 Er1 179.8(9) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C5 C3 C4 118.7(17) . .
C5 C3 N1 109.2(9) . .
C4 C3 N1 109.7(11) . .
C5 C3 H3 106.2 . .
C4 C3 H3 106.2 . .
N1 C3 H3 106.2 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C3 C5 H5A 109.5 . .
C3 C5 H5B 109.5 . .
H5A C5 H5B 109.5 . .
C3 C5 H5C 109.5 . .
H5A C5 H5C 109.5 . .
H5B C5 H5C 109.5 . .
C7 C6 H6A 109.5 . .
C7 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C7 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
N2 C7 C8 106.7(9) . .
N2 C7 C6 124.4(10) . .
C8 C7 C6 129.0(10) . .
C9 C8 C7 106.3(8) . .
C9 C8 H8 126.8 . .
C7 C8 H8 126.8 . .
N3 C9 C8 111.4(9) . .
N3 C9 C10 123.6(8) . .
C8 C9 C10 125.1(8) . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C12 C11 H11A 109.5 . .
C12 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
C12 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
N4 C12 C13 108.6(6) . .
N4 C12 C11 123.4(7) . .
C13 C12 C11 128.0(7) . .
C12 C13 C14 105.9(6) . .
C12 C13 H13 127.0 . .
C14 C13 H13 127.0 . .
N5 C14 C13 110.0(6) . .
N5 C14 C15 122.3(6) . .
C13 C14 C15 127.6(7) . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 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 . .
Si1 C17 H17A 109.5 . .
Si1 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
Si1 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 . .
Si2 C20 H20A 109.5 . .
Si2 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
Si2 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Er1 N6 2.287(7) .
Er1 N1 2.322(5) 4_565
Er1 N1 2.322(5) .
Er1 N5 2.416(5) 4_565
Er1 N5 2.416(5) .
Er1 N3 2.598(7) .
Er1 C1 2.745(10) .
B1 N2 1.535(12) .
B1 N4 1.537(7) 4_565
B1 N4 1.537(7) .
B1 H1 1.18(8) .
Si1 N6 1.736(8) .
Si1 C16 1.860(12) .
Si1 C17 1.881(9) 4_565
Si1 C17 1.881(10) .
Si2 C18 1.711(16) .
Si2 N6 1.719(8) .
Si2 C20 1.762(18) .
Si2 C19 2.18(2) 4_565
Si2 C19 2.18(2) .
N1 C1 1.327(9) .
N1 C3 1.518(13) .
N2 C7 1.350(11) .
N2 N3 1.374(9) .
N3 C9 1.322(11) .
N4 C12 1.346(8) .
N4 N5 1.383(6) .
N5 C14 1.336(8) .
C1 N1 1.327(9) 4_565
C1 C2 1.530(15) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C5 1.467(19) .
C3 C4 1.495(18) .
C3 H3 0.9800 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 H5A 0.9600 .
C5 H5B 0.9600 .
C5 H5C 0.9600 .
C6 C7 1.490(15) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.373(15) .
C8 C9 1.367(14) .
C8 H8 0.9300 .
C9 C10 1.512(14) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.500(9) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.370(10) .
C13 C14 1.388(9) .
C13 H13 0.9300 .
C14 C15 1.503(10) .
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 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
