#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/03/7000308.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_7000308
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           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7680(4)
_cell_length_b                   7.8976(2)
_cell_length_c                   14.2285(5)
_cell_measurement_reflns_used    4973
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.6145
_cell_measurement_theta_min      2.9408
_cell_volume                     2108.98(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  0.0431
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11209
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_exptl_absorpt_coefficient_mu    3.908
_exptl_absorpt_correction_T_max  0.509
_exptl_absorpt_correction_T_min  0.331
_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    1.551
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       drop
_exptl_crystal_F_000             992
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3592
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.950
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0294
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0211P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0482
_refine_ls_wR_factor_ref         0.0521
_reflns_number_gt                2875
_reflns_number_total             3592
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820285k.txt
_cod_data_source_block           CCDC705081
_cod_original_sg_symbol_H-M      Pna21
_cod_database_code               7000308
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.19602(2) 0.22430(5) 0.18506(3) 0.03664(12) Uani 1 1 d . . .
Br2 Br 0.07276(2) 0.25897(5) 0.00727(3) 0.03506(12) Uani 1 1 d . . .
Si1 Si 0.13155(5) 0.41582(13) 0.11065(9) 0.0224(3) Uani 1 1 d . . .
N1 N 0.07345(13) 0.5203(4) 0.1813(3) 0.0228(7) Uani 1 1 d . . .
N2 N 0.18540(15) 0.5630(4) 0.0614(2) 0.0213(7) Uani 1 1 d . . .
C1 C 0.0193(2) 0.7790(5) 0.2395(3) 0.0338(10) Uani 1 1 d . . .
H1A H -0.0090 0.7157 0.2801 0.051 Uiso 1 1 calc R . .
H1B H 0.0154 0.8963 0.2385 0.051 Uiso 1 1 calc R . .
C2 C 0.06654(17) 0.6993(5) 0.1811(3) 0.0223(9) Uani 1 1 d . . .
C3 C 0.11237(18) 0.7947(5) 0.1179(3) 0.0245(10) Uani 1 1 d . . .
H3 H 0.1028 0.9100 0.1137 0.037 Uiso 1 1 calc R . .
C4 C 0.16612(19) 0.7391(5) 0.0652(3) 0.0241(10) Uani 1 1 d . . .
C5 C 0.2095(2) 0.8547(5) 0.0054(3) 0.0332(11) Uani 1 1 d . . .
H5A H 0.1886 0.9656 0.0056 0.050 Uiso 1 1 calc R . .
H5B H 0.2107 0.8120 -0.0578 0.050 Uiso 1 1 calc R . .
H5C H 0.2571 0.8608 0.0297 0.050 Uiso 1 1 calc R . .
C6 C 0.0262(2) 0.4237(5) 0.2412(3) 0.0257(10) Uani 1 1 d . . .
C7 C -0.04105(19) 0.3771(5) 0.2082(3) 0.0260(10) Uani 1 1 d . . .
C8 C -0.0815(2) 0.2648(6) 0.2622(3) 0.0418(12) Uani 1 1 d . . .
H8 H -0.1249 0.2262 0.2392 0.063 Uiso 1 1 calc R . .
C9 C -0.0583(2) 0.2108(6) 0.3480(4) 0.0472(13) Uani 1 1 d . . .
H9 H -0.0857 0.1352 0.3827 0.071 Uiso 1 1 calc R . .
C10 C 0.0058(2) 0.2688(6) 0.3832(3) 0.0422(12) Uani 1 1 d . . .
H10 H 0.0200 0.2362 0.4431 0.063 Uiso 1 1 calc R . .
C11 C 0.0494(2) 0.3752(5) 0.3304(3) 0.0333(11) Uani 1 1 d . . .
C12 C -0.07224(19) 0.4490(5) 0.1199(3) 0.0368(12) Uani 1 1 d . . .
H12A H -0.0363 0.5110 0.0865 0.055 Uiso 1 1 calc R . .
H12B H -0.1109 0.5235 0.1355 0.055 Uiso 1 1 calc R . .
H12C H -0.0896 0.3585 0.0810 0.055 Uiso 1 1 calc R . .
C13 C 0.1176(2) 0.4418(6) 0.3733(3) 0.0495(14) Uani 1 1 d . . .
H13A H 0.1513 0.4653 0.3244 0.074 Uiso 1 1 calc R . .
H13B H 0.1370 0.3584 0.4152 0.074 Uiso 1 1 calc R . .
H13C H 0.1077 0.5438 0.4076 0.074 Uiso 1 1 calc R . .
C14 C 0.25589(18) 0.5198(4) 0.0252(3) 0.0214(10) Uani 1 1 d . . .
C15 C 0.3146(2) 0.5422(5) 0.0837(3) 0.0245(10) Uani 1 1 d . . .
C16 C 0.3813(2) 0.4970(5) 0.0495(3) 0.0360(11) Uani 1 1 d . . .
H16 H 0.4212 0.5091 0.0877 0.054 Uiso 1 1 calc R . .
C17 C 0.3893(2) 0.4345(6) -0.0404(4) 0.0384(12) Uani 1 1 d . . .
H17 H 0.4342 0.4038 -0.0622 0.058 Uiso 1 1 calc R . .
C18 C 0.3316(2) 0.4178(5) -0.0970(3) 0.0334(11) Uani 1 1 d . . .
H18 H 0.3377 0.3766 -0.1576 0.050 Uiso 1 1 calc R . .
C19 C 0.2629(2) 0.4608(5) -0.0667(3) 0.0272(10) Uani 1 1 d . . .
C20 C 0.3072(2) 0.6148(5) 0.1808(3) 0.0357(10) Uani 1 1 d . . .
H20A H 0.2861 0.7253 0.1769 0.054 Uiso 1 1 calc R . .
H20B H 0.3534 0.6233 0.2094 0.054 Uiso 1 1 calc R . .
H20C H 0.2774 0.5422 0.2180 0.054 Uiso 1 1 calc R . .
C21 C 0.2017(2) 0.4444(5) -0.1336(3) 0.0377(11) Uani 1 1 d . . .
H21A H 0.1884 0.3274 -0.1388 0.056 Uiso 1 1 calc R . .
H21B H 0.2156 0.4863 -0.1942 0.056 Uiso 1 1 calc R . .
H21C H 0.1620 0.5089 -0.1106 0.056 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
N2 Si1 N1 107.14(15) . . ?
N2 Si1 Br1 110.00(11) . . ?
N1 Si1 Br1 113.67(13) . . ?
N2 Si1 Br2 113.98(13) . . ?
N1 Si1 Br2 110.16(11) . . ?
Br1 Si1 Br2 102.02(4) . . ?
C2 N1 C6 118.0(3) . . ?
C2 N1 Si1 122.8(3) . . ?
C6 N1 Si1 119.1(2) . . ?
C4 N2 C14 117.9(3) . . ?
C4 N2 Si1 119.9(2) . . ?
C14 N2 Si1 121.8(2) . . ?
C1 C2 N1 121.1(4) . . ?
C1 C2 C3 121.4(4) . . ?
N1 C2 C3 117.6(3) . . ?
C4 C3 C2 128.7(4) . . ?
C3 C4 N2 122.1(4) . . ?
C3 C4 C5 122.3(3) . . ?
N2 C4 C5 115.7(3) . . ?
C11 C6 C7 121.1(4) . . ?
C11 C6 N1 119.3(4) . . ?
C7 C6 N1 119.6(4) . . ?
C6 C7 C8 118.2(4) . . ?
C6 C7 C12 122.4(4) . . ?
C8 C7 C12 119.3(4) . . ?
C9 C8 C7 121.2(4) . . ?
C8 C9 C10 119.9(4) . . ?
C9 C10 C11 121.1(4) . . ?
C10 C11 C6 118.2(4) . . ?
C10 C11 C13 119.3(4) . . ?
C6 C11 C13 122.4(4) . . ?
C15 C14 C19 121.9(3) . . ?
C15 C14 N2 118.4(3) . . ?
C19 C14 N2 119.7(3) . . ?
C16 C15 C14 118.1(4) . . ?
C16 C15 C20 120.3(4) . . ?
C14 C15 C20 121.7(3) . . ?
C17 C16 C15 121.0(4) . . ?
C18 C17 C16 120.0(4) . . ?
C17 C18 C19 121.9(4) . . ?
C14 C19 C18 117.2(4) . . ?
C14 C19 C21 123.5(3) . . ?
C18 C19 C21 119.3(4) . . ?
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
Br1 Si1 2.2074(11) . ?
Br2 Si1 2.2171(12) . ?
Si1 N2 1.692(3) . ?
Si1 N1 1.697(3) . ?
N1 C2 1.419(5) . ?
N1 C6 1.448(5) . ?
N2 C4 1.438(5) . ?
N2 C14 1.460(4) . ?
C1 C2 1.369(5) . ?
C2 C3 1.455(5) . ?
C3 C4 1.331(5) . ?
C4 C5 1.490(6) . ?
C6 C11 1.396(6) . ?
C6 C7 1.396(5) . ?
C7 C8 1.397(5) . ?
C7 C12 1.497(5) . ?
C8 C9 1.364(6) . ?
C9 C10 1.381(6) . ?
C10 C11 1.392(6) . ?
C11 C13 1.512(5) . ?
C14 C15 1.393(5) . ?
C14 C19 1.394(5) . ?
C15 C16 1.391(5) . ?
C15 C20 1.501(5) . ?
C16 C17 1.378(6) . ?
C17 C18 1.356(6) . ?
C18 C19 1.400(5) . ?
C19 C21 1.497(5) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652571
