#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/42/7014255.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_7014255
loop_
_publ_author_name
'Hitchcock, Peter B.'
'Hu, Jin'
'Lappert, Michael F.'
'Severn, John R.'
_publ_section_title
;
 Synthesis and structures of beta-diketiminatotin(II) halides, an amide
 and of Sn(=E)[{N(R)C(Ph)}2CH](NR2) (E = S or Se, R = SiMe3).
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4193
_journal_page_last               4201
_journal_paper_doi               10.1039/b412765j
_journal_year                    2004
_chemical_formula_sum            'C21 H29 Br0.6 Cl0.4 N2 Si2 Sn'
_chemical_formula_weight         546.64
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.87(2)
_cell_angle_beta                 100.23(1)
_cell_angle_gamma                104.26(2)
_cell_formula_units_Z            2
_cell_length_a                   6.434(1)
_cell_length_b                   11.986(4)
_cell_length_c                   17.262(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      10
_cell_measurement_theta_min      7
_cell_volume                     1242.0(5)
_computing_cell_refinement       'Nonius CAD4 software'
_computing_data_collection       'Nonius CAD4 software'
_computing_data_reduction        'Nonius CAD4 software'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius CAD4'
_diffrn_measurement_method       'omega-2theta scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0643
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5978
_diffrn_reflns_theta_full        27.97
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.37
_exptl_absorpt_coefficient_mu    2.148
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.77
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   psi-scans
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.848
_refine_diff_density_min         -0.533
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5978
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0287P)²+0.4596P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.1005
_reflns_number_gt                4008
_reflns_number_total             5978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b412765j.txt
_cod_data_source_block           (3)-jun1095
_cod_original_sg_symbol_H-M      P-1
_cod_original_formula_sum        'C21 H29 Br0.60 Cl0.40 N2 Si2 Sn'
_cod_database_code               7014255
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
Sn Sn 0.27851(5) 0.62822(3) 0.696454(18) 0.05355(12) Uani 1 1 d . . .
Br Br 0.67442(10) 0.75222(7) 0.75537(5) 0.0790(3) Uani 0.604(4) 1 d P . .
Cl Cl 0.67442(10) 0.75222(7) 0.75537(5) 0.0790(3) Uani 0.396(4) 1 d P . .
Si1 Si 0.04535(18) 0.53256(9) 0.84118(7) 0.0433(3) Uani 1 1 d . . .
Si2 Si 0.02370(19) 0.76721(11) 0.57276(6) 0.0524(3) Uani 1 1 d . . .
N2 N 0.1748(5) 0.7810(3) 0.67194(17) 0.0406(7) Uani 1 1 d . . .
N1 N 0.1873(5) 0.6595(2) 0.81157(18) 0.0395(7) Uani 1 1 d . . .
C1 C 0.2326(6) 0.7710(3) 0.8502(2) 0.0365(8) Uani 1 1 d . . .
C2 C 0.2690(6) 0.8686(3) 0.8147(2) 0.0410(9) Uani 1 1 d . . .
H2 H 0.3330 0.9410 0.8499 0.049 Uiso 1 1 calc R . .
C3 C 0.2222(6) 0.8720(3) 0.7335(2) 0.0369(8) Uani 1 1 d . . .
C4 C 0.2503(7) 0.7961(3) 0.9387(2) 0.0443(9) Uani 1 1 d . . .
C5 C 0.4039(7) 0.7615(4) 0.9896(3) 0.0538(10) Uani 1 1 d . . .
H5 H 0.4950 0.7218 0.9683 0.065 Uiso 1 1 calc R . .
C9 C 0.1169(9) 0.8553(4) 0.9722(3) 0.0627(12) Uani 1 1 d . . .
H9 H 0.0154 0.8808 0.9391 0.075 Uiso 1 1 calc R . .
C6 C 0.4216(9) 0.7858(4) 1.0717(3) 0.0716(14) Uani 1 1 d . . .
H6 H 0.5269 0.7635 1.1053 0.086 Uiso 1 1 calc R . .
C7 C 0.2878(11) 0.8416(5) 1.1042(3) 0.0811(17) Uani 1 1 d . . .
H7 H 0.2998 0.8563 1.1595 0.097 Uiso 1 1 calc R . .
C8 C 0.1338(11) 0.8765(4) 1.0544(3) 0.0842(17) Uani 1 1 d . . .
H8 H 0.0411 0.9143 1.0763 0.101 Uiso 1 1 calc R . .
C10 C 0.2336(6) 0.9919(3) 0.7164(2) 0.0415(9) Uani 1 1 d . . .
C11 C 0.0986(8) 1.0554(4) 0.7425(2) 0.0554(11) Uani 1 1 d . . .
H11 H -0.0025 1.0238 0.7713 0.066 Uiso 1 1 calc R . .
C12 C 0.1128(10) 1.1659(4) 0.7260(3) 0.0731(14) Uani 1 1 d . . .
H12 H 0.0179 1.2074 0.7421 0.088 Uiso 1 1 calc R . .
C13 C 0.2668(10) 1.2144(4) 0.6860(3) 0.0754(16) Uani 1 1 d . . .
H13 H 0.2777 1.2894 0.6758 0.091 Uiso 1 1 calc R . .
C14 C 0.4036(9) 1.1535(4) 0.6610(3) 0.0698(14) Uani 1 1 d . . .
H14 H 0.5083 1.1872 0.6343 0.084 Uiso 1 1 calc R . .
C15 C 0.3879(7) 1.0412(4) 0.6753(2) 0.0546(11) Uani 1 1 d . . .
H15 H 0.4802 0.9993 0.6574 0.066 Uiso 1 1 calc R . .
C16 C -0.1512(8) 0.4376(4) 0.7483(3) 0.0705(14) Uani 1 1 d . . .
H16A H -0.0716 0.4205 0.7081 0.106 Uiso 1 1 calc R . .
H16B H -0.2546 0.4779 0.7285 0.106 Uiso 1 1 calc R . .
H16C H -0.2287 0.3655 0.7606 0.106 Uiso 1 1 calc R . .
C17 C 0.2426(7) 0.4524(4) 0.8781(3) 0.0597(12) Uani 1 1 d . . .
H17A H 0.3263 0.4387 0.8386 0.090 Uiso 1 1 calc R . .
H17B H 0.1631 0.3785 0.8873 0.090 Uiso 1 1 calc R . .
H17C H 0.3403 0.4987 0.9275 0.090 Uiso 1 1 calc R . .
C18 C -0.1204(7) 0.5613(4) 0.9152(3) 0.0608(12) Uani 1 1 d . . .
H18A H -0.2208 0.6027 0.8946 0.091 Uiso 1 1 calc R . .
H18B H -0.0246 0.6081 0.9648 0.091 Uiso 1 1 calc R . .
H18C H -0.2018 0.4879 0.9246 0.091 Uiso 1 1 calc R . .
C19 C -0.1356(8) 0.8752(5) 0.5618(3) 0.0712(14) Uani 1 1 d . . .
H19A H -0.2338 0.8695 0.5978 0.107 Uiso 1 1 calc R . .
H19B H -0.2193 0.8589 0.5074 0.107 Uiso 1 1 calc R . .
H19C H -0.0365 0.9531 0.5744 0.107 Uiso 1 1 calc R . .
C20 C 0.2153(9) 0.7757(6) 0.5039(3) 0.099(2) Uani 1 1 d . . .
H20A H 0.2965 0.7192 0.5104 0.148 Uiso 1 1 calc R . .
H20B H 0.3157 0.8533 0.5163 0.148 Uiso 1 1 calc R . .
H20C H 0.1329 0.7591 0.4493 0.148 Uiso 1 1 calc R . .
C21 C -0.1776(9) 0.6192(4) 0.5453(3) 0.0802(16) Uani 1 1 d . . .
H21A H -0.1009 0.5605 0.5503 0.120 Uiso 1 1 calc R . .
H21B H -0.2585 0.6060 0.4908 0.120 Uiso 1 1 calc R . .
H21C H -0.2776 0.6145 0.5807 0.120 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'
Br Br -0.2901 2.4595 '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'
Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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 Sn N1 87.35(11) . . ?
N2 Sn Br 91.98(9) . . ?
N1 Sn Br 92.53(8) . . ?
N1 Si1 C18 114.52(17) . . ?
N1 Si1 C17 109.60(18) . . ?
C18 Si1 C17 111.2(2) . . ?
N1 Si1 C16 105.95(19) . . ?
C18 Si1 C16 106.7(2) . . ?
C17 Si1 C16 108.5(2) . . ?
N2 Si2 C19 114.65(19) . . ?
N2 Si2 C20 108.8(2) . . ?
C19 Si2 C20 110.6(3) . . ?
N2 Si2 C21 106.4(2) . . ?
C19 Si2 C21 107.0(3) . . ?
C20 Si2 C21 109.2(3) . . ?
C3 N2 Si2 127.3(3) . . ?
C3 N2 Sn 116.8(2) . . ?
Si2 N2 Sn 115.83(15) . . ?
C1 N1 Si1 126.9(3) . . ?
C1 N1 Sn 117.5(2) . . ?
Si1 N1 Sn 115.53(15) . . ?
N1 C1 C2 125.3(3) . . ?
N1 C1 C4 118.8(3) . . ?
C2 C1 C4 115.9(3) . . ?
C3 C2 C1 128.5(3) . . ?
N2 C3 C2 126.4(3) . . ?
N2 C3 C10 118.9(3) . . ?
C2 C3 C10 114.8(3) . . ?
C9 C4 C5 118.6(4) . . ?
C9 C4 C1 121.2(4) . . ?
C5 C4 C1 120.2(4) . . ?
C6 C5 C4 120.2(5) . . ?
C8 C9 C4 120.4(5) . . ?
C7 C6 C5 121.1(5) . . ?
C6 C7 C8 119.5(5) . . ?
C7 C8 C9 120.3(5) . . ?
C11 C10 C15 119.4(4) . . ?
C11 C10 C3 121.4(3) . . ?
C15 C10 C3 119.2(4) . . ?
C10 C11 C12 120.2(4) . . ?
C13 C12 C11 120.0(5) . . ?
C14 C13 C12 120.3(5) . . ?
C13 C14 C15 120.4(5) . . ?
C14 C15 C10 119.6(5) . . ?
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
Sn N2 2.172(3) . ?
Sn N1 2.174(3) . ?
Sn Br 2.5457(10) . ?
Si1 N1 1.770(3) . ?
Si1 C18 1.848(4) . ?
Si1 C17 1.855(4) . ?
Si1 C16 1.863(5) . ?
Si2 N2 1.774(3) . ?
Si2 C19 1.850(5) . ?
Si2 C20 1.855(5) . ?
Si2 C21 1.855(5) . ?
N2 C3 1.333(4) . ?
N1 C1 1.334(4) . ?
C1 C2 1.391(5) . ?
C1 C4 1.489(5) . ?
C2 C3 1.389(5) . ?
C3 C10 1.498(5) . ?
C4 C9 1.387(6) . ?
C4 C5 1.388(6) . ?
C5 C6 1.381(6) . ?
C9 C8 1.383(6) . ?
C6 C7 1.358(7) . ?
C7 C8 1.381(8) . ?
C10 C11 1.377(6) . ?
C10 C15 1.390(5) . ?
C11 C12 1.382(6) . ?
C12 C13 1.372(7) . ?
C13 C14 1.359(7) . ?
C14 C15 1.387(6) . ?
