#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/59/4325920.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_4325920
loop_
_publ_author_name
'Dongming Yang'
'Yuqiang Ding'
'Haishun Wu'
'Wenjun Zheng'
_publ_section_title
;
 Synthesis and Structural Characterization of Alkaline-Earth-Metal
 Bis(amido)silane and Lithium Oxobis(aminolato)silane Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7698
_journal_page_last               7706
_journal_paper_doi               10.1021/ic200748z
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C21 H36 Ba0.5 N O2 Si0.5'
_chemical_formula_weight         417.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 108.854(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.606(3)
_cell_length_b                   10.127(3)
_cell_length_c                   22.487(6)
_cell_measurement_reflns_used    878
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.252
_cell_measurement_theta_min      2.797
_cell_volume                     2285.7(11)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0481
_diffrn_reflns_av_sigmaI/netI    0.0503
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            7792
_diffrn_reflns_theta_full        23.29
_diffrn_reflns_theta_max         23.29
_diffrn_reflns_theta_min         1.91
_exptl_absorpt_coefficient_mu    0.932
_exptl_absorpt_correction_T_max  0.8728
_exptl_absorpt_correction_T_min  0.8141
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       block
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.003
_refine_diff_density_min         -0.422
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.975
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3294
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.975
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0434
_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)+(0.0666P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1026
_refine_ls_wR_factor_ref         0.1068
_reflns_number_gt                2779
_reflns_number_total             3294
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200748z_si_002_4.cif
_cod_data_source_block           a00701a
_cod_original_cell_volume        2285.7(12)
_cod_original_formula_sum        'C21 H36 Ba0.50 N O2 Si0.50'
_cod_database_code               4325920
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
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
Ba1 Ba 0.5000 0.46126(4) 0.2500 0.05500(17) Uani 1 2 d S
Si1 Si 0.5000 0.1400(2) 0.2500 0.0951(9) Uani 1 2 d S
N1 N 0.5886(4) 0.2426(4) 0.30741(16) 0.0636(10) Uani 1 1 d .
C1 C 0.3982(10) 0.0198(9) 0.2789(4) 0.232(8) Uani 1 1 d .
H1A H 0.4226 -0.0687 0.2720 0.348 Uiso 1 1 calc R
H1B H 0.3054 0.0334 0.2566 0.348 Uiso 1 1 calc R
H1C H 0.4147 0.0333 0.3231 0.348 Uiso 1 1 calc R
C2 C 0.6648(5) 0.2028(4) 0.3680(2) 0.0568(12) Uani 1 1 d .
C3 C 0.6102(5) 0.1978(5) 0.4169(2) 0.0691(14) Uani 1 1 d .
C4 C 0.6892(6) 0.1651(6) 0.4768(2) 0.0860(17) Uani 1 1 d .
H4A H 0.6516 0.1630 0.5088 0.103 Uiso 1 1 calc R
C5 C 0.8209(6) 0.1356(7) 0.4905(3) 0.0942(19) Uani 1 1 d .
H5A H 0.8719 0.1123 0.5312 0.113 Uiso 1 1 calc R
C6 C 0.8765(5) 0.1407(6) 0.4440(2) 0.0812(16) Uani 1 1 d .
H6A H 0.9669 0.1227 0.4535 0.097 Uiso 1 1 calc R
C7 C 0.8020(5) 0.1719(5) 0.3828(2) 0.0633(12) Uani 1 1 d .
C8 C 0.8706(6) 0.1764(7) 0.3338(3) 0.0909(18) Uani 1 1 d .
H8A H 0.8013 0.1877 0.2929 0.109 Uiso 1 1 calc R
C9 C 0.9448(10) 0.0460(9) 0.3309(4) 0.147(4) Uani 1 1 d .
H9A H 0.8841 -0.0268 0.3249 0.221 Uiso 1 1 calc R
H9B H 1.0168 0.0343 0.3695 0.221 Uiso 1 1 calc R
H9C H 0.9796 0.0498 0.2965 0.221 Uiso 1 1 calc R
C10 C 0.9637(9) 0.2902(10) 0.3425(4) 0.169(4) Uani 1 1 d .
H10A H 0.9166 0.3708 0.3431 0.253 Uiso 1 1 calc R
H10B H 0.9997 0.2926 0.3084 0.253 Uiso 1 1 calc R
H10C H 1.0350 0.2805 0.3815 0.253 Uiso 1 1 calc R
C11 C 0.4663(6) 0.2342(8) 0.4075(3) 0.103(2) Uani 1 1 d .
H11A H 0.4206 0.2428 0.3622 0.124 Uiso 1 1 calc R
C12 C 0.3935(7) 0.1300(11) 0.4323(4) 0.171(4) Uani 1 1 d .
H12A H 0.3031 0.1574 0.4249 0.256 Uiso 1 1 calc R
H12B H 0.4371 0.1187 0.4766 0.256 Uiso 1 1 calc R
H12C H 0.3943 0.0478 0.4111 0.256 Uiso 1 1 calc R
C13 C 0.4566(10) 0.3640(11) 0.4372(4) 0.170(4) Uani 1 1 d .
H13A H 0.5019 0.4303 0.4213 0.255 Uiso 1 1 calc R
H13B H 0.4971 0.3571 0.4820 0.255 Uiso 1 1 calc R
H13C H 0.3646 0.3880 0.4276 0.255 Uiso 1 1 calc R
O1 O 0.6778(5) 0.5971(5) 0.3556(2) 0.1254(17) Uani 1 1 d .
C14 C 0.7597(15) 0.5440(9) 0.4098(6) 0.239(8) Uani 1 1 d .
H14A H 0.7076 0.4895 0.4287 0.286 Uiso 1 1 calc R
H14B H 0.8245 0.4876 0.4002 0.286 Uiso 1 1 calc R
C15 C 0.8249(11) 0.6371(11) 0.4518(4) 0.196(5) Uani 1 1 d .
H15A H 0.9205 0.6244 0.4636 0.235 Uiso 1 1 calc R
H15B H 0.7990 0.6329 0.4894 0.235 Uiso 1 1 calc R
C16 C 0.7884(14) 0.7576(11) 0.4216(6) 0.219(6) Uani 1 1 d .
H16A H 0.7403 0.8109 0.4430 0.263 Uiso 1 1 calc R
H16B H 0.8663 0.8061 0.4203 0.263 Uiso 1 1 calc R
C17 C 0.7079(13) 0.7253(10) 0.3619(6) 0.263(9) Uani 1 1 d .
H17A H 0.6262 0.7761 0.3519 0.316 Uiso 1 1 calc R
H17B H 0.7527 0.7494 0.3321 0.316 Uiso 1 1 calc R
O2 O 0.6814(5) 0.5755(4) 0.2002(2) 0.1065(14) Uani 1 1 d .
C18 C 0.7992(8) 0.5183(10) 0.1965(5) 0.147(3) Uani 1 1 d .
H18A H 0.7823 0.4313 0.1776 0.177 Uiso 1 1 calc R
H18B H 0.8656 0.5110 0.2378 0.177 Uiso 1 1 calc R
C19 C 0.8440(10) 0.6142(13) 0.1551(6) 0.189(5) Uani 1 1 d .
H19A H 0.9404 0.6204 0.1689 0.227 Uiso 1 1 calc R
H19B H 0.8129 0.5853 0.1117 0.227 Uiso 1 1 calc R
C20 C 0.7884(11) 0.7351(10) 0.1613(5) 0.168(4) Uani 1 1 d .
H20A H 0.7696 0.7872 0.1232 0.202 Uiso 1 1 calc R
H20B H 0.8463 0.7850 0.1964 0.202 Uiso 1 1 calc R
C21 C 0.6713(13) 0.6978(8) 0.1723(8) 0.255(9) Uani 1 1 d .
H21A H 0.6500 0.7629 0.1992 0.305 Uiso 1 1 calc R
H21B H 0.5989 0.6965 0.1327 0.305 Uiso 1 1 calc R
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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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'
Ba Ba -0.3244 2.2819 '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 Ba1 N1 61.93(15) 2_655 .
N1 Ba1 O2 111.84(14) 2_655 2_655
N1 Ba1 O2 110.10(13) . 2_655
N1 Ba1 O2 110.10(13) 2_655 .
N1 Ba1 O2 111.84(14) . .
O2 Ba1 O2 130.67(19) 2_655 .
N1 Ba1 O1 149.60(14) 2_655 .
N1 Ba1 O1 87.80(14) . .
O2 Ba1 O1 79.69(16) 2_655 .
O2 Ba1 O1 77.17(16) . .
N1 Ba1 O1 87.80(14) 2_655 2_655
N1 Ba1 O1 149.60(14) . 2_655
O2 Ba1 O1 77.17(16) 2_655 2_655
O2 Ba1 O1 79.69(16) . 2_655
O1 Ba1 O1 122.6(2) . 2_655
N1 Ba1 Si1 30.97(8) 2_655 .
N1 Ba1 Si1 30.97(8) . .
O2 Ba1 Si1 114.66(9) 2_655 .
O2 Ba1 Si1 114.66(9) . .
O1 Ba1 Si1 118.72(12) . .
O1 Ba1 Si1 118.72(12) 2_655 .
N1 Si1 N1 104.0(3) . 2_655
N1 Si1 C1 112.0(3) . .
N1 Si1 C1 115.1(3) 2_655 .
N1 Si1 C1 115.1(3) . 2_655
N1 Si1 C1 112.0(3) 2_655 2_655
C1 Si1 C1 99.2(8) . 2_655
N1 Si1 Ba1 51.98(13) . .
N1 Si1 Ba1 51.98(13) 2_655 .
C1 Si1 Ba1 130.4(4) . .
C1 Si1 Ba1 130.4(4) 2_655 .
C2 N1 Si1 124.8(3) . .
C2 N1 Ba1 137.4(3) . .
Si1 N1 Ba1 97.06(15) . .
Si1 C1 H1A 109.5 . .
Si1 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
Si1 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
N1 C2 C3 121.3(4) . .
N1 C2 C7 121.1(4) . .
C3 C2 C7 117.5(4) . .
C4 C3 C2 120.1(5) . .
C4 C3 C11 117.6(5) . .
C2 C3 C11 122.3(4) . .
C5 C4 C3 122.1(5) . .
C5 C4 H4A 119.0 . .
C3 C4 H4A 119.0 . .
C6 C5 C4 119.1(5) . .
C6 C5 H5A 120.5 . .
C4 C5 H5A 120.5 . .
C5 C6 C7 121.6(5) . .
C5 C6 H6A 119.2 . .
C7 C6 H6A 119.2 . .
C6 C7 C2 119.7(5) . .
C6 C7 C8 118.7(5) . .
C2 C7 C8 121.6(4) . .
C10 C8 C7 112.7(6) . .
C10 C8 C9 109.9(7) . .
C7 C8 C9 112.2(5) . .
C10 C8 H8A 107.3 . .
C7 C8 H8A 107.3 . .
C9 C8 H8A 107.3 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C8 C10 H10A 109.5 . .
C8 C10 H10B 109.5 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C13 C11 C3 111.3(7) . .
C13 C11 C12 109.3(7) . .
C3 C11 C12 112.8(6) . .
C13 C11 H11A 107.7 . .
C3 C11 H11A 107.7 . .
C12 C11 H11A 107.7 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C17 O1 C14 103.2(6) . .
C17 O1 Ba1 128.8(5) . .
C14 O1 Ba1 127.8(5) . .
C15 C14 O1 112.6(8) . .
C15 C14 H14A 109.1 . .
O1 C14 H14A 109.1 . .
C15 C14 H14B 109.1 . .
O1 C14 H14B 109.1 . .
H14A C14 H14B 107.8 . .
C14 C15 C16 105.8(9) . .
C14 C15 H15A 110.6 . .
C16 C15 H15A 110.6 . .
C14 C15 H15B 110.6 . .
C16 C15 H15B 110.6 . .
H15A C15 H15B 108.7 . .
C17 C16 C15 104.8(8) . .
C17 C16 H16A 110.8 . .
C15 C16 H16A 110.8 . .
C17 C16 H16B 110.8 . .
C15 C16 H16B 110.8 . .
H16A C16 H16B 108.9 . .
O1 C17 C16 112.7(9) . .
O1 C17 H17A 109.1 . .
C16 C17 H17A 109.1 . .
O1 C17 H17B 109.1 . .
C16 C17 H17B 109.1 . .
H17A C17 H17B 107.8 . .
C21 O2 C18 106.6(6) . .
C21 O2 Ba1 126.7(5) . .
C18 O2 Ba1 126.7(4) . .
O2 C18 C19 103.4(7) . .
O2 C18 H18A 111.1 . .
C19 C18 H18A 111.1 . .
O2 C18 H18B 111.1 . .
C19 C18 H18B 111.1 . .
H18A C18 H18B 109.1 . .
C20 C19 C18 105.9(8) . .
C20 C19 H19A 110.5 . .
C18 C19 H19A 110.5 . .
C20 C19 H19B 110.5 . .
C18 C19 H19B 110.5 . .
H19A C19 H19B 108.7 . .
C19 C20 C21 102.2(9) . .
C19 C20 H20A 111.3 . .
C21 C20 H20A 111.3 . .
C19 C20 H20B 111.3 . .
C21 C20 H20B 111.3 . .
H20A C20 H20B 109.2 . .
O2 C21 C20 112.4(9) . .
O2 C21 H21A 109.1 . .
C20 C21 H21A 109.1 . .
O2 C21 H21B 109.1 . .
C20 C21 H21B 109.1 . .
H21A C21 H21B 107.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 N1 2.582(4) 2_655
Ba1 N1 2.582(4) .
Ba1 O2 2.774(4) 2_655
Ba1 O2 2.774(4) .
Ba1 O1 2.863(4) .
Ba1 O1 2.863(4) 2_655
Ba1 Si1 3.253(2) .
Si1 N1 1.687(4) .
Si1 N1 1.687(4) 2_655
Si1 C1 1.877(8) .
Si1 C1 1.877(8) 2_655
N1 C2 1.400(5) .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 C3 1.400(7) .
C2 C7 1.419(6) .
C3 C4 1.377(7) .
C3 C11 1.516(7) .
C4 C5 1.362(8) .
C4 H4A 0.9300 .
C5 C6 1.357(8) .
C5 H5A 0.9300 .
C6 C7 1.385(7) .
C6 H6A 0.9300 .
C7 C8 1.504(7) .
C8 C10 1.489(10) .
C8 C9 1.550(9) .
C8 H8A 0.9800 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C11 C13 1.494(12) .
C11 C12 1.517(10) .
C11 H11A 0.9800 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
O1 C17 1.333(10) .
O1 C14 1.359(11) .
C14 C15 1.355(11) .
C14 H14A 0.9700 .
C14 H14B 0.9700 .
C15 C16 1.389(13) .
C15 H15A 0.9700 .
C15 H15B 0.9700 .
C16 C17 1.378(12) .
C16 H16A 0.9700 .
C16 H16B 0.9700 .
C17 H17A 0.9700 .
C17 H17B 0.9700 .
O2 C21 1.376(10) .
O2 C18 1.403(9) .
C18 C19 1.524(12) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.386(13) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 C21 1.394(12) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
