#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/03/7000306.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_7000306
loop_
_publ_author_name
'Xiong, Yun'
'Yao, Shenglai'
'Driess, Matthias'
_publ_section_title
;
 Twice silicon-induced C--H activation and tautomerisation of a
 β-diketiminato ligand and formation of new types of N-heterocyclic
 silanes
;
_journal_issue                   3
_journal_name_full               'Dalton Transactions'
_journal_page_first              421
_journal_page_last               423
_journal_paper_doi               10.1039/b820285k
_journal_year                    2009
_chemical_formula_sum            'C21 H24 Br2 N2 Si'
_chemical_formula_weight         492.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.903(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.9450(4)
_cell_length_b                   8.2720(2)
_cell_length_c                   17.7852(4)
_cell_measurement_reflns_used    5635
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.7107
_cell_measurement_theta_min      2.9217
_cell_volume                     2124.74(10)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
;
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur S Sapphire'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0452
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13787
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_exptl_absorpt_coefficient_mu    3.879
_exptl_absorpt_correction_T_max  0.750
_exptl_absorpt_correction_T_min  0.358
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET)
(compiled Apr 13 2006,12:24:59)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.438
_refine_diff_density_min         -0.400
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0305
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0351P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0630
_refine_ls_wR_factor_ref         0.0708
_reflns_number_gt                2656
_reflns_number_total             3731
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820285k.txt
_cod_data_source_block           CCDC705079
_cod_original_cell_volume        2124.73(9)
_cod_original_sg_symbol_H-M      P21/a
_cod_database_code               7000306
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x-1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Si1 Si 0.20271(6) 0.58350(11) 0.23187(5) 0.0187(2) Uani 1 1 d . . .
Br1 Br 0.16249(3) 0.40161(4) 0.137393(19) 0.03375(12) Uani 1 1 d . . .
Br2 Br 0.35648(2) 0.58292(5) 0.249717(19) 0.03318(12) Uani 1 1 d . . .
N1 N 0.15653(17) 0.7695(3) 0.20082(13) 0.0173(6) Uani 1 1 d . . .
N2 N 0.08605(18) 0.6222(3) 0.41115(14) 0.0234(7) Uani 1 1 d . . .
H2 H 0.0595 0.7013 0.4282 0.035 Uiso 1 1 calc R . .
C1 C 0.0838(2) 1.0298(4) 0.21802(19) 0.0320(9) Uani 1 1 d . . .
H1A H 0.0558 1.0828 0.2542 0.048 Uiso 1 1 calc R . .
H1B H 0.0398 1.0227 0.1682 0.048 Uiso 1 1 calc R . .
H1C H 0.1367 1.0906 0.2131 0.048 Uiso 1 1 calc R . .
C2 C 0.1136(2) 0.8641(4) 0.24674(17) 0.0195(7) Uani 1 1 d . . .
C3 C 0.0981(2) 0.8096(4) 0.31409(17) 0.0208(7) Uani 1 1 d . . .
H3 H 0.0717 0.8822 0.3421 0.031 Uiso 1 1 calc R . .
C4 C 0.1185(2) 0.6504(4) 0.34668(17) 0.0187(7) Uani 1 1 d . . .
C5 C 0.1674(2) 0.5378(4) 0.31757(17) 0.0221(8) Uani 1 1 d . . .
H5 H 0.1820 0.4386 0.3422 0.033 Uiso 1 1 calc R . .
C6 C 0.0928(2) 0.4734(4) 0.45186(18) 0.0228(8) Uani 1 1 d . . .
C7 C 0.0407(2) 0.3407(4) 0.41701(19) 0.0278(8) Uani 1 1 d . . .
C8 C 0.0484(3) 0.1981(4) 0.4590(2) 0.0337(9) Uani 1 1 d . . .
H8 H 0.0149 0.1076 0.4368 0.051 Uiso 1 1 calc R . .
C9 C 0.1057(3) 0.1890(5) 0.5337(2) 0.0380(10) Uani 1 1 d . . .
H9 H 0.1111 0.0920 0.5610 0.057 Uiso 1 1 calc R . .
C10 C 0.1542(2) 0.3222(5) 0.5676(2) 0.0331(9) Uani 1 1 d . . .
H10 H 0.1907 0.3155 0.6185 0.050 Uiso 1 1 calc R . .
C11 C 0.1500(2) 0.4662(4) 0.52754(19) 0.0251(8) Uani 1 1 d . . .
C12 C -0.0247(2) 0.3541(5) 0.33694(19) 0.0355(9) Uani 1 1 d . . .
H12A H 0.0103 0.3614 0.2988 0.053 Uiso 1 1 calc R . .
H12B H -0.0623 0.4490 0.3344 0.053 Uiso 1 1 calc R . .
H12C H -0.0638 0.2602 0.3268 0.053 Uiso 1 1 calc R . .
C13 C 0.2048(2) 0.6118(5) 0.56418(19) 0.0381(10) Uani 1 1 d . . .
H13A H 0.2428 0.6487 0.5316 0.057 Uiso 1 1 calc R . .
H13B H 0.2433 0.5830 0.6144 0.057 Uiso 1 1 calc R . .
H13C H 0.1631 0.6964 0.5699 0.057 Uiso 1 1 calc R . .
C14 C 0.1533(2) 0.8242(4) 0.12225(17) 0.0213(8) Uani 1 1 d . . .
C15 C 0.0755(2) 0.7843(4) 0.06265(18) 0.0265(8) Uani 1 1 d . . .
C16 C 0.0758(3) 0.8263(5) -0.01299(19) 0.0389(10) Uani 1 1 d . . .
H16 H 0.0259 0.7970 -0.0539 0.058 Uiso 1 1 calc R . .
C17 C 0.1482(3) 0.9102(5) -0.0282(2) 0.0412(10) Uani 1 1 d . . .
H17 H 0.1475 0.9354 -0.0793 0.062 Uiso 1 1 calc R . .
C18 C 0.2218(3) 0.9572(4) 0.0314(2) 0.0369(10) Uani 1 1 d . . .
H18 H 0.2696 1.0172 0.0204 0.055 Uiso 1 1 calc R . .
C19 C 0.2258(2) 0.9162(4) 0.10811(18) 0.0255(8) Uani 1 1 d . . .
C20 C -0.0085(2) 0.7015(5) 0.0777(2) 0.0373(10) Uani 1 1 d . . .
H20A H -0.0297 0.6190 0.0393 0.056 Uiso 1 1 calc R . .
H20B H -0.0568 0.7795 0.0747 0.056 Uiso 1 1 calc R . .
H20C H 0.0077 0.6535 0.1285 0.056 Uiso 1 1 calc R . .
C21 C 0.3051(2) 0.9776(4) 0.1722(2) 0.0363(9) Uani 1 1 d . . .
H21A H 0.2905 0.9647 0.2214 0.055 Uiso 1 1 calc R . .
H21B H 0.3153 1.0899 0.1637 0.055 Uiso 1 1 calc R . .
H21C H 0.3600 0.9173 0.1724 0.055 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
N1 Si1 C5 106.41(14) . . ?
N1 Si1 Br1 110.82(9) . . ?
C5 Si1 Br1 115.00(11) . . ?
N1 Si1 Br2 111.14(9) . . ?
C5 Si1 Br2 113.50(11) . . ?
Br1 Si1 Br2 100.03(4) . . ?
C2 N1 C14 118.6(2) . . ?
C2 N1 Si1 121.3(2) . . ?
C14 N1 Si1 119.8(2) . . ?
C4 N2 C6 125.4(3) . . ?
C3 C2 N1 122.5(3) . . ?
C3 C2 C1 120.4(3) . . ?
N1 C2 C1 117.1(3) . . ?
C2 C3 C4 126.5(3) . . ?
C5 C4 N2 122.5(3) . . ?
C5 C4 C3 123.4(3) . . ?
N2 C4 C3 114.1(3) . . ?
C4 C5 Si1 119.1(2) . . ?
C7 C6 C11 121.8(3) . . ?
C7 C6 N2 119.8(3) . . ?
C11 C6 N2 118.3(3) . . ?
C8 C7 C6 118.1(3) . . ?
C8 C7 C12 121.0(3) . . ?
C6 C7 C12 120.9(3) . . ?
C7 C8 C9 120.6(4) . . ?
C10 C9 C8 120.3(3) . . ?
C9 C10 C11 121.1(3) . . ?
C10 C11 C6 118.0(3) . . ?
C10 C11 C13 121.2(3) . . ?
C6 C11 C13 120.8(3) . . ?
C15 C14 C19 121.6(3) . . ?
C15 C14 N1 118.1(3) . . ?
C19 C14 N1 120.3(3) . . ?
C16 C15 C14 117.8(3) . . ?
C16 C15 C20 119.5(3) . . ?
C14 C15 C20 122.6(3) . . ?
C17 C16 C15 121.1(3) . . ?
C16 C17 C18 120.5(3) . . ?
C17 C18 C19 120.7(3) . . ?
C18 C19 C14 118.0(3) . . ?
C18 C19 C21 119.1(3) . . ?
C14 C19 C21 122.9(3) . . ?
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 1.718(3) . ?
Si1 C5 1.777(3) . ?
Si1 Br1 2.2201(9) . ?
Si1 Br2 2.2375(9) . ?
N1 C2 1.401(4) . ?
N1 C14 1.458(4) . ?
N2 C4 1.375(4) . ?
N2 C6 1.418(4) . ?
C1 C2 1.490(4) . ?
C2 C3 1.354(4) . ?
C3 C4 1.439(4) . ?
C4 C5 1.365(4) . ?
C6 C7 1.396(5) . ?
C6 C11 1.398(4) . ?
C7 C8 1.385(5) . ?
C7 C12 1.510(5) . ?
C8 C9 1.385(5) . ?
C9 C10 1.372(5) . ?
C10 C11 1.381(5) . ?
C11 C13 1.507(5) . ?
C14 C15 1.396(4) . ?
C14 C19 1.399(4) . ?
C15 C16 1.390(4) . ?
C15 C20 1.513(4) . ?
C16 C17 1.370(5) . ?
C17 C18 1.374(5) . ?
C18 C19 1.393(4) . ?
C19 C21 1.506(4) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652569
