#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:20:52 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179408 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/05/4330583.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_4330583
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 N9 Si2 Y'
_chemical_formula_weight         687.74
_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                 110.937(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.715(8)
_cell_length_b                   14.056(9)
_cell_length_c                   12.208(8)
_cell_measurement_reflns_used    923
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.057
_cell_measurement_theta_min      2.359
_cell_volume                     1878(2)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0479
_diffrn_reflns_av_sigmaI/netI    0.0449
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7747
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.648
_exptl_absorpt_correction_T_max  0.8794
_exptl_absorpt_correction_T_min  0.7340
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.217
_exptl_crystal_description       block
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.882
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3453
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0726
_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)+(0.0057P)²+15.8428P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1677
_refine_ls_wR_factor_ref         0.1720
_reflns_number_gt                2967
_reflns_number_total             3453
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3008552_si_001_2.cif
_cod_data_source_block           a01102c
_cod_original_cell_volume        1877(2)
_cod_database_code               4330583
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
Y1 Y 0.18809(7) 0.2500 0.17759(7) 0.0322(2) Uani 1 2 d S
B1 B 0.1972(9) 0.2500 -0.1079(9) 0.049(3) Uani 1 2 d S
Si1 Si 0.5167(2) 0.2500 0.3136(3) 0.0620(9) Uani 1 2 d S
Si2 Si 0.3807(3) 0.2500 0.4700(3) 0.115(2) Uani 1 2 d SU
N1 N 0.0468(5) 0.3293(6) 0.2401(6) 0.073(2) Uani 1 1 d .
N2 N 0.0606(6) 0.2500 -0.1237(6) 0.0435(18) Uani 1 2 d S
N3 N 0.0231(6) 0.2500 -0.0303(6) 0.0407(17) Uani 1 2 d S
N4 N 0.2569(4) 0.1581(4) -0.0432(4) 0.0428(12) Uani 1 1 d .
N5 N 0.2559(4) 0.1338(4) 0.0657(4) 0.0408(12) Uani 1 1 d .
N6 N 0.3762(6) 0.2500 0.3287(7) 0.050(2) Uani 1 2 d S
C1 C -0.0013(10) 0.2500 0.2613(11) 0.087(5) Uani 1 2 d S
C2 C -0.1075(13) 0.2500 0.3078(15) 0.170(11) Uani 1 2 d S
H2A H -0.1372 0.1862 0.3070 0.254 Uiso 0.50 1 calc PR
H2B H -0.1723 0.2897 0.2588 0.254 Uiso 0.50 1 calc PR
H2C H -0.0792 0.2740 0.3866 0.254 Uiso 0.50 1 calc PR
C3 C -0.0060(12) 0.4225(12) 0.2448(13) 0.152(7) Uani 1 1 d .
H3 H -0.0924 0.4113 0.2321 0.183 Uiso 1 1 calc R
C4 C 0.0490(19) 0.4672(16) 0.3648(15) 0.34(2) Uani 1 1 d .
H4A H 0.0440 0.4232 0.4230 0.515 Uiso 1 1 calc R
H4B H 0.0049 0.5241 0.3676 0.515 Uiso 1 1 calc R
H4C H 0.1331 0.4826 0.3799 0.515 Uiso 1 1 calc R
C5 C -0.0040(11) 0.4829(10) 0.1454(16) 0.177(9) Uani 1 1 d .
H5A H 0.0742 0.4773 0.1370 0.265 Uiso 1 1 calc R
H5B H -0.0180 0.5481 0.1605 0.265 Uiso 1 1 calc R
H5C H -0.0669 0.4623 0.0744 0.265 Uiso 1 1 calc R
C6 C -0.0259(13) 0.2500 -0.3447(10) 0.104(6) Uani 1 2 d S
H6A H -0.0245 0.3144 -0.3704 0.156 Uiso 0.50 1 calc PR
H6B H -0.0949 0.2174 -0.3991 0.156 Uiso 0.50 1 calc PR
H6C H 0.0480 0.2182 -0.3410 0.156 Uiso 0.50 1 calc PR
C7 C -0.0355(9) 0.2500 -0.2267(9) 0.063(3) Uani 1 2 d S
C8 C -0.1381(9) 0.2500 -0.1995(9) 0.062(3) Uani 1 2 d S
H8 H -0.2183 0.2500 -0.2523 0.074 Uiso 1 2 calc SR
C9 C -0.1011(8) 0.2500 -0.0783(9) 0.047(2) Uani 1 2 d S
C10 C -0.1832(9) 0.2500 -0.0093(11) 0.078(4) Uani 1 2 d S
H10A H -0.1833 0.1879 0.0235 0.117 Uiso 0.50 1 calc PR
H10B H -0.2647 0.2661 -0.0597 0.117 Uiso 0.50 1 calc PR
H10C H -0.1547 0.2959 0.0528 0.117 Uiso 0.50 1 calc PR
C11 C 0.3270(9) 0.0905(8) -0.1979(8) 0.094(3) Uani 1 1 d .
H11A H 0.2486 0.0876 -0.2599 0.141 Uiso 1 1 calc R
H11B H 0.3755 0.0370 -0.2035 0.141 Uiso 1 1 calc R
H11C H 0.3677 0.1483 -0.2046 0.141 Uiso 1 1 calc R
C12 C 0.3104(7) 0.0885(6) -0.0825(7) 0.0578(19) Uani 1 1 d .
C13 C 0.3437(7) 0.0177(6) 0.0007(8) 0.069(2) Uani 1 1 d .
H13 H 0.3813 -0.0398 -0.0036 0.082 Uiso 1 1 calc R
C14 C 0.3097(6) 0.0494(5) 0.0923(7) 0.0543(18) Uani 1 1 d .
C15 C 0.3275(7) 0.0003(6) 0.2057(7) 0.073(2) Uani 1 1 d .
H15A H 0.3202 0.0457 0.2616 0.109 Uiso 1 1 calc R
H15B H 0.4072 -0.0281 0.2351 0.109 Uiso 1 1 calc R
H15C H 0.2665 -0.0482 0.1934 0.109 Uiso 1 1 calc R
C16 C 0.5165(10) 0.2500 0.1611(11) 0.118(7) Uani 1 2 d S
H16A H 0.4812 0.1918 0.1228 0.177 Uiso 0.50 1 calc PR
H16B H 0.5989 0.2553 0.1630 0.177 Uiso 0.50 1 calc PR
H16C H 0.4693 0.3029 0.1187 0.177 Uiso 0.50 1 calc PR
C17 C 0.6126(8) 0.3564(8) 0.3822(9) 0.098(3) Uani 1 1 d .
H17A H 0.5650 0.4133 0.3569 0.147 Uiso 1 1 calc R
H17B H 0.6825 0.3588 0.3588 0.147 Uiso 1 1 calc R
H17C H 0.6392 0.3515 0.4661 0.147 Uiso 1 1 calc R
C18 C 0.2512(14) 0.2500 0.5042(12) 0.193(14) Uani 1 2 d S
H18A H 0.2193 0.3135 0.4978 0.289 Uiso 0.50 1 calc PR
H18B H 0.2704 0.2275 0.5830 0.289 Uiso 0.50 1 calc PR
H18C H 0.1912 0.2090 0.4510 0.289 Uiso 0.50 1 calc PR
C19 C 0.378(3) 0.100(2) 0.5066(17) 0.160(10) Uani 0.50 1 d PU
H19A H 0.3062 0.0714 0.4501 0.240 Uiso 0.50 1 calc PR
H19B H 0.3756 0.0913 0.5839 0.240 Uiso 0.50 1 calc PR
H19C H 0.4494 0.0701 0.5020 0.240 Uiso 0.50 1 calc PR
C20 C 0.5170(15) 0.2500 0.5921(12) 0.26(2) Uani 1 2 d S
H20A H 0.5498 0.3133 0.6056 0.395 Uiso 0.50 1 calc PR
H20B H 0.5749 0.2082 0.5777 0.395 Uiso 0.50 1 calc PR
H20C H 0.5010 0.2285 0.6598 0.395 Uiso 0.50 1 calc PR
H1 H 0.207(9) 0.2500 -0.206(9) 0.07(3) 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'
Y Y -2.7962 3.5667 '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 Y1 N1 108.8(2) . 4_565
N6 Y1 N1 108.8(2) . .
N1 Y1 N1 57.0(4) 4_565 .
N6 Y1 N5 92.22(19) . .
N1 Y1 N5 105.9(2) 4_565 .
N1 Y1 N5 155.9(2) . .
N6 Y1 N5 92.22(19) . 4_565
N1 Y1 N5 155.9(2) 4_565 4_565
N1 Y1 N5 105.9(2) . 4_565
N5 Y1 N5 84.2(3) . 4_565
N6 Y1 N3 161.5(2) . .
N1 Y1 N3 87.3(2) 4_565 .
N1 Y1 N3 87.3(2) . .
N5 Y1 N3 74.25(16) . .
N5 Y1 N3 74.25(16) 4_565 .
N6 Y1 C1 111.6(3) . .
N1 Y1 C1 28.5(2) 4_565 .
N1 Y1 C1 28.5(2) . .
N5 Y1 C1 132.45(16) . .
N5 Y1 C1 132.45(16) 4_565 .
N3 Y1 C1 86.9(3) . .
N2 B1 N4 108.9(5) . 4_565
N2 B1 N4 108.9(5) . .
N4 B1 N4 113.5(7) 4_565 .
N2 B1 H1 109(5) . .
N4 B1 H1 108(2) 4_565 .
N4 B1 H1 108(2) . .
N6 Si1 C16 116.6(4) . .
N6 Si1 C17 113.2(3) . .
C16 Si1 C17 103.5(4) . .
N6 Si1 C17 113.2(3) . 4_565
C16 Si1 C17 103.5(4) . 4_565
C17 Si1 C17 105.6(7) . 4_565
N6 Si2 C18 122.4(6) . .
N6 Si2 C20 123.3(7) . .
C18 Si2 C20 114.3(8) . .
N6 Si2 C19 102.2(5) . .
C18 Si2 C19 82.4(6) . .
C20 Si2 C19 84.4(7) . .
N6 Si2 C19 102.2(5) . 4_565
C18 Si2 C19 82.4(6) . 4_565
C20 Si2 C19 84.4(7) . 4_565
C19 Si2 C19 155.4(10) . 4_565
C1 N1 C3 122.4(9) . .
C1 N1 Y1 93.6(6) . .
C3 N1 Y1 143.2(9) . .
C7 N2 N3 111.6(8) . .
C7 N2 B1 126.7(8) . .
N3 N2 B1 121.7(7) . .
C9 N3 N2 104.8(7) . .
C9 N3 Y1 137.1(6) . .
N2 N3 Y1 118.1(5) . .
C12 N4 N5 109.3(6) . .
C12 N4 B1 127.8(6) . .
N5 N4 B1 122.8(6) . .
C14 N5 N4 106.9(5) . .
C14 N5 Y1 133.1(5) . .
N4 N5 Y1 119.5(4) . .
Si2 N6 Si1 115.0(4) . .
Si2 N6 Y1 118.8(4) . .
Si1 N6 Y1 126.1(4) . .
N1 C1 N1 115.9(10) . 4_565
N1 C1 C2 122.1(5) . .
N1 C1 C2 122.1(5) 4_565 .
N1 C1 Y1 57.9(5) . .
N1 C1 Y1 57.9(5) 4_565 .
C2 C1 Y1 179.8(10) . .
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 . .
N1 C3 C5 110.5(11) . .
N1 C3 C4 111.8(11) . .
C5 C3 C4 115.3(18) . .
N1 C3 H3 106.2 . .
C5 C3 H3 106.2 . .
C4 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 125.1(10) . .
C8 C7 C6 128.2(10) . .
C7 C8 C9 107.2(9) . .
C7 C8 H8 126.4 . .
C9 C8 H8 126.4 . .
N3 C9 C8 109.8(9) . .
N3 C9 C10 124.4(9) . .
C8 C9 C10 125.9(9) . .
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 108.1(6) . .
N4 C12 C11 124.1(8) . .
C13 C12 C11 127.8(7) . .
C12 C13 C14 106.0(7) . .
C12 C13 H13 127.0 . .
C14 C13 H13 127.0 . .
N5 C14 C13 109.7(7) . .
N5 C14 C15 122.4(7) . .
C13 C14 C15 127.8(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
Y1 N6 2.314(7) .
Y1 N1 2.339(6) 4_565
Y1 N1 2.339(6) .
Y1 N5 2.437(5) .
Y1 N5 2.437(5) 4_565
Y1 N3 2.582(7) .
Y1 C1 2.755(11) .
B1 N2 1.541(12) .
B1 N4 1.544(8) 4_565
B1 N4 1.544(8) .
B1 H1 1.24(10) .
Si1 N6 1.721(8) .
Si1 C16 1.862(13) .
Si1 C17 1.878(9) .
Si1 C17 1.878(9) 4_565
Si2 N6 1.707(9) .
Si2 C18 1.711(15) .
Si2 C20 1.752(14) .
Si2 C19 2.16(3) .
Si2 C19 2.16(3) 4_565
N1 C1 1.316(9) .
N1 C3 1.458(14) .
N2 C7 1.355(11) .
N2 N3 1.361(10) .
N3 C9 1.361(11) .
N4 C12 1.340(8) .
N4 N5 1.377(7) .
N5 C14 1.329(9) .
C1 N1 1.316(9) 4_565
C1 C2 1.541(16) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C5 1.49(2) .
C3 C4 1.509(17) .
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 1.484(15) .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C7 C8 1.357(15) .
C8 C9 1.385(14) .
C8 H8 0.9300 .
C9 C10 1.487(14) .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C12 1.490(10) .
C11 H11A 0.9600 .
C11 H11B 0.9600 .
C11 H11C 0.9600 .
C12 C13 1.376(11) .
C13 C14 1.388(10) .
C13 H13 0.9300 .
C14 C15 1.493(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 .
