#------------------------------------------------------------------------------
#$Date: 2017-10-14 22:27:35 +0300 (Sat, 14 Oct 2017) $
#$Revision: 202017 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/00/03/7000307.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_7000307
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 H23 Br5 N2 Si2'
_chemical_formula_weight         759.14
_chemical_name_systematic
;
?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 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                   11.1177(5)
_cell_length_b                   13.9333(7)
_cell_length_c                   16.9301(6)
_cell_measurement_reflns_used    4022
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.4768
_cell_measurement_theta_min      3.0170
_cell_volume                     2622.6(2)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0687
_diffrn_reflns_av_sigmaI/netI    0.1168
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13453
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    7.766
_exptl_absorpt_correction_T_max  0.451
_exptl_absorpt_correction_T_min  0.149
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET)
(compiled Aug 28 2006,13:05:05)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.923
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1464
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.118
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.005(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.910
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     276
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.910
_refine_ls_R_factor_all          0.0787
_refine_ls_R_factor_gt           0.0410
_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)+(0.0221P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0611
_refine_ls_wR_factor_ref         0.0690
_reflns_number_gt                3015
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b820285k.txt
_cod_data_source_block           CCDC705080
_cod_original_sg_symbol_H-M      P212121
_cod_database_code               7000307
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'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
Br1 Br 0.42957(7) 0.07879(7) 0.20453(5) 0.0362(2) Uani 1 1 d . . .
Br2 Br 0.60629(7) -0.09076(7) 0.29724(5) 0.0330(2) Uani 1 1 d . . .
Br3 Br -0.07076(8) -0.06907(7) 0.45913(5) 0.0430(3) Uani 1 1 d . . .
Br4 Br 0.07355(8) -0.27529(6) 0.52730(5) 0.0364(2) Uani 1 1 d . . .
Br5 Br -0.12586(7) -0.29157(7) 0.36611(5) 0.0403(3) Uani 1 1 d . . .
Si1 Si 0.42442(19) -0.02427(16) 0.30465(12) 0.0240(5) Uani 1 1 d . . .
Si2 Si 0.01401(18) -0.20267(17) 0.41976(12) 0.0236(6) Uani 1 1 d . . .
N1 N 0.4009(5) 0.0335(4) 0.3929(3) 0.0180(15) Uani 1 1 d . . .
N2 N 0.1238(5) -0.1846(4) 0.3514(3) 0.0223(16) Uani 1 1 d . . .
C1 C 0.3246(6) 0.0389(6) 0.5297(4) 0.025(2) Uani 1 1 d . . .
H1A H 0.2699 0.0039 0.5648 0.038 Uiso 1 1 calc R . .
H1B H 0.2996 0.1063 0.5267 0.038 Uiso 1 1 calc R . .
H1C H 0.4067 0.0353 0.5506 0.038 Uiso 1 1 calc R . .
C2 C 0.3210(7) -0.0046(6) 0.4493(4) 0.022(2) Uani 1 1 d . . .
C3 C 0.2447(6) -0.0784(6) 0.4332(4) 0.0211(19) Uani 1 1 d . . .
H3 H 0.1981 -0.1025 0.4758 0.032 Uiso 1 1 calc R . .
C4 C 0.2281(6) -0.1228(6) 0.3579(4) 0.019(2) Uani 1 1 d . . .
C5 C 0.3032(6) -0.1090(5) 0.2967(5) 0.0212(19) Uani 1 1 d . . .
H5 H 0.2922 -0.1441 0.2492 0.032 Uiso 1 1 calc R . .
C6 C 0.4515(6) 0.1299(6) 0.4087(4) 0.0183(19) Uani 1 1 d . . .
C7 C 0.3807(6) 0.2098(6) 0.3890(4) 0.0193(18) Uani 1 1 d . . .
C8 C 0.4285(7) 0.3001(6) 0.3999(4) 0.025(2) Uani 1 1 d . . .
H8 H 0.3815 0.3552 0.3881 0.038 Uiso 1 1 calc R . .
C9 C 0.5435(8) 0.3110(6) 0.4278(4) 0.031(2) Uani 1 1 d . . .
H9 H 0.5767 0.3736 0.4325 0.046 Uiso 1 1 calc R . .
C10 C 0.6124(7) 0.2313(6) 0.4494(4) 0.026(2) Uani 1 1 d . . .
H10 H 0.6912 0.2402 0.4699 0.039 Uiso 1 1 calc R . .
C11 C 0.5668(7) 0.1400(6) 0.4409(4) 0.0175(18) Uani 1 1 d . . .
C12 C 0.2550(6) 0.1981(7) 0.3572(4) 0.034(2) Uani 1 1 d . . .
H12A H 0.2581 0.1649 0.3062 0.051 Uiso 1 1 calc R . .
H12B H 0.2181 0.2614 0.3502 0.051 Uiso 1 1 calc R . .
H12C H 0.2070 0.1603 0.3944 0.051 Uiso 1 1 calc R . .
C13 C 0.6384(6) 0.0565(6) 0.4720(5) 0.031(2) Uani 1 1 d . . .
H13A H 0.6993 0.0381 0.4330 0.046 Uiso 1 1 calc R . .
H13B H 0.5845 0.0022 0.4818 0.046 Uiso 1 1 calc R . .
H13C H 0.6780 0.0750 0.5214 0.046 Uiso 1 1 calc R . .
C14 C 0.1140(6) -0.2324(6) 0.2751(4) 0.0194(19) Uani 1 1 d . . .
C15 C 0.0541(6) -0.1856(5) 0.2142(4) 0.0210(19) Uani 1 1 d . . .
C16 C 0.0439(6) -0.2345(6) 0.1417(4) 0.028(2) Uani 1 1 d . . .
H16 H 0.0028 -0.2049 0.0989 0.042 Uiso 1 1 calc R . .
C17 C 0.0926(7) -0.3246(6) 0.1320(5) 0.030(2) Uani 1 1 d . . .
H17 H 0.0866 -0.3560 0.0824 0.045 Uiso 1 1 calc R . .
C18 C 0.1510(6) -0.3698(6) 0.1949(4) 0.025(2) Uani 1 1 d . . .
H18 H 0.1814 -0.4330 0.1882 0.038 Uiso 1 1 calc R . .
C19 C 0.1651(6) -0.3242(6) 0.2665(4) 0.019(2) Uani 1 1 d . . .
C20 C 0.0005(7) -0.0889(6) 0.2261(4) 0.031(2) Uani 1 1 d . . .
H20A H -0.0792 -0.0956 0.2502 0.047 Uiso 1 1 calc R . .
H20B H -0.0071 -0.0565 0.1750 0.047 Uiso 1 1 calc R . .
H20C H 0.0525 -0.0510 0.2609 0.047 Uiso 1 1 calc R . .
C21 C 0.2287(7) -0.3726(6) 0.3343(4) 0.028(2) Uani 1 1 d . . .
H21A H 0.1709 -0.3858 0.3766 0.041 Uiso 1 1 calc R . .
H21B H 0.2923 -0.3304 0.3543 0.041 Uiso 1 1 calc R . .
H21C H 0.2642 -0.4330 0.3160 0.041 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 105.0(3) . . ?
N1 Si1 Br1 111.4(2) . . ?
C5 Si1 Br1 112.8(3) . . ?
N1 Si1 Br2 112.5(2) . . ?
C5 Si1 Br2 113.8(3) . . ?
Br1 Si1 Br2 101.68(9) . . ?
N2 Si2 Br4 114.7(2) . . ?
N2 Si2 Br5 108.2(2) . . ?
Br4 Si2 Br5 107.41(10) . . ?
N2 Si2 Br3 113.0(2) . . ?
Br4 Si2 Br3 105.68(9) . . ?
Br5 Si2 Br3 107.58(9) . . ?
C2 N1 C6 117.3(6) . . ?
C2 N1 Si1 120.6(5) . . ?
C6 N1 Si1 121.7(5) . . ?
C4 N2 C14 113.5(5) . . ?
C4 N2 Si2 127.7(5) . . ?
C14 N2 Si2 118.8(5) . . ?
C3 C2 N1 122.8(7) . . ?
C3 C2 C1 120.5(7) . . ?
N1 C2 C1 116.7(7) . . ?
C2 C3 C4 125.9(7) . . ?
C5 C4 C3 123.0(7) . . ?
C5 C4 N2 121.6(7) . . ?
C3 C4 N2 115.3(6) . . ?
C4 C5 Si1 120.2(6) . . ?
C11 C6 C7 121.8(7) . . ?
C11 C6 N1 120.6(7) . . ?
C7 C6 N1 117.6(6) . . ?
C8 C7 C6 118.4(7) . . ?
C8 C7 C12 120.3(7) . . ?
C6 C7 C12 121.3(7) . . ?
C9 C8 C7 120.5(8) . . ?
C8 C9 C10 120.9(8) . . ?
C11 C10 C9 120.3(7) . . ?
C10 C11 C6 118.1(7) . . ?
C10 C11 C13 118.9(7) . . ?
C6 C11 C13 122.9(7) . . ?
C15 C14 C19 122.9(7) . . ?
C15 C14 N2 118.6(7) . . ?
C19 C14 N2 118.5(6) . . ?
C14 C15 C16 117.2(7) . . ?
C14 C15 C20 121.1(7) . . ?
C16 C15 C20 121.6(7) . . ?
C17 C16 C15 120.9(8) . . ?
C16 C17 C18 120.2(8) . . ?
C19 C18 C17 121.0(8) . . ?
C18 C19 C14 117.7(7) . . ?
C18 C19 C21 121.1(7) . . ?
C14 C19 C21 121.2(7) . . ?
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 2.222(2) . ?
Br2 Si1 2.228(2) . ?
Br3 Si2 2.190(2) . ?
Br4 Si2 2.186(2) . ?
Br5 Si2 2.186(2) . ?
Si1 N1 1.717(6) . ?
Si1 C5 1.796(7) . ?
Si2 N2 1.701(6) . ?
N1 C2 1.410(9) . ?
N1 C6 1.481(9) . ?
N2 C4 1.448(8) . ?
N2 C14 1.457(8) . ?
C1 C2 1.491(9) . ?
C2 C3 1.360(10) . ?
C3 C4 1.429(9) . ?
C4 C5 1.344(9) . ?
C6 C11 1.400(10) . ?
C6 C7 1.404(9) . ?
C7 C8 1.378(10) . ?
C7 C12 1.507(9) . ?
C8 C9 1.371(10) . ?
C9 C10 1.398(10) . ?
C10 C11 1.377(9) . ?
C11 C13 1.504(10) . ?
C14 C15 1.390(9) . ?
C14 C19 1.407(10) . ?
C15 C16 1.409(9) . ?
C15 C20 1.486(10) . ?
C16 C17 1.377(10) . ?
C17 C18 1.398(9) . ?
C18 C19 1.378(9) . ?
C19 C21 1.507(9) . ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 ChemSpider 30652570
