#------------------------------------------------------------------------------
#$Date: 2019-11-24 23:02:09 +0200 (Sun, 24 Nov 2019) $
#$Revision: 239674 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/69/4516988.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_4516988
loop_
_publ_author_name
'Wirtz, Lisa'
'Jourdain, Matthias'
'Huch, Volker'
'Zimmer, Michael'
'Schäfer, André'
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Disiloxa[3]tetrelocenophanes.
;
_journal_issue                   19
_journal_name_full               'ACS omega'
_journal_page_first              18355
_journal_page_last               18360
_journal_paper_doi               10.1021/acsomega.9b02605
_journal_volume                  4
_journal_year                    2019
_chemical_formula_moiety         'C21 H32 N2 O Si2 Sn'
_chemical_formula_sum            'C21 H32 N2 O Si2 Sn'
_chemical_formula_weight         503.35
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.7562(6)
_cell_length_b                   12.0231(5)
_cell_length_c                   11.4859(4)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    142(2)
_cell_measurement_theta_max      35.67
_cell_measurement_theta_min      2.45
_cell_volume                     2313.97(15)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      142(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0370
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26404
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         36.638
_diffrn_reflns_theta_min         2.150
_exptl_absorpt_coefficient_mu    1.221
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6827
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.445
_exptl_crystal_description       pillar
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.682
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.116
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.087
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5875
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0247
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0275P)²+0.0977P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0535
_refine_ls_wR_factor_ref         0.0574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4827
_reflns_number_total             5875
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ao9b02605_si_006.cif
_cod_data_source_block           sh4042
_cod_database_code               4516988
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Sn Sn 0.64116(2) 0.2500 0.38107(2) 0.01426(3) Uani 1 2 d S T P
Si Si 0.84801(2) 0.38080(3) 0.31990(3) 0.01494(6) Uani 1 1 d . . .
O O 0.86081(7) 0.2500 0.35450(11) 0.0194(2) Uani 1 2 d S T P
N1 N 0.56805(9) 0.2500 0.65803(13) 0.0195(3) Uani 1 2 d S T P
N2 N 0.69485(9) 0.2500 0.67608(12) 0.0189(3) Uani 1 2 d S T P
C1 C 0.74139(6) 0.41914(9) 0.32011(10) 0.01607(19) Uani 1 1 d . . .
C2 C 0.69477(7) 0.45014(9) 0.42008(10) 0.0179(2) Uani 1 1 d . . .
C3 C 0.61812(8) 0.48100(10) 0.38290(11) 0.0210(2) Uani 1 1 d . . .
C4 C 0.61598(7) 0.47202(11) 0.26064(11) 0.0219(2) Uani 1 1 d . . .
C5 C 0.69030(7) 0.43486(10) 0.22243(10) 0.0190(2) Uani 1 1 d . . .
C6 C 0.90151(8) 0.46101(11) 0.43332(12) 0.0237(2) Uani 1 1 d . . .
C7 C 0.89188(9) 0.40815(14) 0.17448(12) 0.0278(3) Uani 1 1 d . . .
C8 C 0.63626(10) 0.2500 0.59488(15) 0.0189(3) Uani 1 2 d S T P
C9 C 0.58340(11) 0.2500 0.77686(14) 0.0208(3) Uani 1 2 d S T P
C10 C 0.66367(12) 0.2500 0.78850(15) 0.0214(3) Uani 1 2 d S T P
C11 C 0.48799(12) 0.2500 0.60795(17) 0.0279(4) Uani 1 2 d S T P
H11A H 0.4640 0.1762 0.6173 0.042 Uiso 0.5 1 calc R U P
H11B H 0.4912 0.2685 0.5250 0.042 Uiso 0.5 1 calc R U P
H11C H 0.4550 0.3054 0.6480 0.042 Uiso 0.5 1 calc R U P
C12 C 0.51790(14) 0.2500 0.86503(17) 0.0305(4) Uani 1 2 d S T P
H12A H 0.5406 0.2388 0.9428 0.046 Uiso 0.5 1 calc R U P
H12B H 0.4804 0.1897 0.8476 0.046 Uiso 0.5 1 calc R U P
H12C H 0.4898 0.3214 0.8625 0.046 Uiso 0.5 1 calc R U P
C13 C 0.71607(14) 0.2500 0.89297(16) 0.0315(4) Uani 1 2 d S T P
H13A H 0.7560 0.3092 0.8856 0.047 Uiso 0.5 1 calc R U P
H13B H 0.7431 0.1779 0.8994 0.047 Uiso 0.5 1 calc R U P
H13C H 0.6837 0.2629 0.9628 0.047 Uiso 0.5 1 calc R U P
C14 C 0.77971(11) 0.2500 0.65023(17) 0.0256(3) Uani 1 2 d S T P
H14A H 0.8055 0.3116 0.6915 0.038 Uiso 0.5 1 calc R U P
H14B H 0.7876 0.2590 0.5662 0.038 Uiso 0.5 1 calc R U P
H14C H 0.8033 0.1794 0.6756 0.038 Uiso 0.5 1 calc R U P
H4 H 0.7042(9) 0.4204(13) 0.1448(14) 0.023(4) Uiso 1 1 d . . .
H1 H 0.7133(9) 0.4538(12) 0.4957(13) 0.024(4) Uiso 1 1 d . . .
H3 H 0.5699(9) 0.4862(14) 0.2120(14) 0.030(4) Uiso 1 1 d . . .
H2 H 0.5759(9) 0.5065(13) 0.4293(14) 0.025(4) Uiso 1 1 d . . .
H8 H 0.9452(12) 0.3799(16) 0.1707(17) 0.047(5) Uiso 1 1 d . . .
H5 H 0.9569(10) 0.4441(14) 0.4368(14) 0.031(4) Uiso 1 1 d . . .
H6 H 0.8832(11) 0.4457(16) 0.5041(17) 0.042(5) Uiso 1 1 d . . .
H9 H 0.8619(10) 0.3655(18) 0.1153(15) 0.037(6) Uiso 1 1 d . . .
H7 H 0.8949(11) 0.5356(17) 0.4233(16) 0.042(5) Uiso 1 1 d . . .
H10 H 0.8871(12) 0.4895(19) 0.1606(19) 0.051(5) Uiso 1 1 d . . .
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'
Sn Sn -0.6537 1.4246 '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
C8 Sn C2 80.78(3) . 7_565
C8 Sn C2 80.78(3) . .
C2 Sn C2 134.71(5) 7_565 .
O Si C1 111.52(5) . .
O Si C6 105.43(6) . .
C1 Si C6 109.74(6) . .
O Si C7 109.71(7) . .
C1 Si C7 109.92(6) . .
C6 Si C7 110.44(7) . .
Si O Si 147.96(9) 7_565 .
C8 N1 C9 111.72(15) . .
C8 N1 C11 124.39(15) . .
C9 N1 C11 123.88(15) . .
C8 N2 C10 111.50(15) . .
C8 N2 C14 124.67(15) . .
C10 N2 C14 123.82(15) . .
C5 C1 C2 105.55(10) . .
C5 C1 Si 127.91(9) . .
C2 C1 Si 126.29(9) . .
C3 C2 C1 108.83(10) . .
C3 C2 Sn 82.90(7) . .
C1 C2 Sn 79.09(6) . .
C3 C2 H1 125.5(9) . .
C1 C2 H1 125.5(9) . .
Sn C2 H1 108.7(9) . .
C2 C3 C4 107.84(11) . .
C2 C3 H2 127.2(10) . .
C4 C3 H2 124.9(10) . .
C5 C4 C3 108.40(11) . .
C5 C4 H3 126.0(9) . .
C3 C4 H3 125.6(9) . .
C4 C5 C1 109.37(10) . .
C4 C5 H4 125.5(10) . .
C1 C5 H4 125.1(10) . .
Si C6 H5 113.0(10) . .
Si C6 H6 111.7(12) . .
H5 C6 H6 104.7(15) . .
Si C6 H7 111.4(12) . .
H5 C6 H7 109.6(15) . .
H6 C6 H7 106.1(16) . .
Si C7 H8 110.4(12) . .
Si C7 H9 109.0(10) . .
H8 C7 H9 105.0(15) . .
Si C7 H10 106.6(12) . .
H8 C7 H10 114.7(16) . .
H9 C7 H10 111.0(17) . .
N1 C8 N2 104.07(14) . .
N1 C8 Sn 124.31(12) . .
N2 C8 Sn 131.62(12) . .
C10 C9 N1 106.35(15) . .
C10 C9 C12 131.63(17) . .
N1 C9 C12 122.02(17) . .
C9 C10 N2 106.35(15) . .
C9 C10 C13 131.87(17) . .
N2 C10 C13 121.78(17) . .
N1 C11 H11A 109.5 . .
N1 C11 H11B 109.5 . .
H11A C11 H11B 109.5 . .
N1 C11 H11C 109.5 . .
H11A C11 H11C 109.5 . .
H11B C11 H11C 109.5 . .
C9 C12 H12A 109.5 . .
C9 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C9 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C10 C13 H13A 109.5 . .
C10 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C10 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
N2 C14 H14A 109.5 . .
N2 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
N2 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn C8 2.4572(17) .
Sn C2 2.6072(11) 7_565
Sn C2 2.6073(11) .
Si O 1.6362(5) .
Si C1 1.8450(11) .
Si C6 1.8522(13) .
Si C7 1.8544(13) .
O Si 1.6362(5) 7_565
N1 C8 1.354(2) .
N1 C9 1.389(2) .
N1 C11 1.460(2) .
N2 C8 1.354(2) .
N2 C10 1.393(2) .
N2 C14 1.453(2) .
C1 C5 1.4239(15) .
C1 C2 1.4380(16) .
C2 C3 1.4035(17) .
C2 H1 0.923(15) .
C3 C4 1.4088(18) .
C3 H2 0.937(15) .
C4 C5 1.3939(17) .
C4 H3 0.969(16) .
C5 H4 0.938(15) .
C6 H5 0.951(17) .
C6 H6 0.89(2) .
C6 H7 0.91(2) .
C7 H8 0.957(19) .
C7 H9 0.989(19) .
C7 H10 0.99(2) .
C9 C10 1.352(3) .
C9 C12 1.493(3) .
C10 C13 1.487(3) .
C11 H11A 0.9800 .
C11 H11B 0.9800 .
C11 H11C 0.9800 .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C12 H12C 0.9800 .
C13 H13A 0.9800 .
C13 H13B 0.9800 .
C13 H13C 0.9800 .
C14 H14A 0.9800 .
C14 H14B 0.9800 .
C14 H14C 0.9800 .
