#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:11:05 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179049 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/11/4301109.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_4301109
loop_
_publ_author_name
'Herbert W. Roesky'
'Anukul Jana'
'Carola Schulzke'
'Alexander Döring'
'Tobias Beck'
'Aritra Pal'
'Regine Herbst-Irmer'
_publ_contact_author_address
;Institut für Anorganische Chemie
der Georg-August-Universität Göttingen
Tammannstr. 4, 37077 Göttingen, Germany
;
_publ_contact_author_email       hroesky@gwdg.de
_publ_contact_author_fax         +49-551-393373
_publ_contact_author_name        'Herbert W. Roesky'
_publ_contact_author_phone       +49-551-393001
_publ_section_title
;
Facile Access of Stable Divalent Tin Compounds with Terminal Methyl, Amide,
Fluoride, and Iodide Substituents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              193
_journal_page_last               197
_journal_paper_doi               10.1021/ic8015639
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C30 H44 N2 Sn'
_chemical_formula_weight         551.36
_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                98.08(3)
_cell_angle_beta                 98.62(3)
_cell_angle_gamma                105.76(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6420(17)
_cell_length_b                   11.638(2)
_cell_length_c                   14.986(3)
_cell_measurement_reflns_used    13371
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      54.3
_cell_measurement_theta_min      3.7
_cell_volume                     1407.9(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device_type  IPDS2
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0436
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13371
_diffrn_reflns_theta_full        27.14
_diffrn_reflns_theta_max         27.14
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    0.926
_exptl_absorpt_correction_T_max  0.9199
_exptl_absorpt_correction_T_min  0.7792
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.705
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     312
_refine_ls_number_reflns         6051
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0295
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0342P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0606
_refine_ls_wR_factor_ref         0.0636
_reflns_number_gt                5195
_reflns_number_total             6051
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8015639_si_002_2.cif
_cod_data_source_block           comp2
_cod_original_cell_volume        1407.9(5)
_cod_database_code               4301109
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
Sn1 Sn -0.04458(2) 0.060930(16) 0.733251(13) 0.02065(6) Uani 1 1 d . . .
N1 N 0.0576(2) -0.08295(17) 0.77370(13) 0.0177(4) Uani 1 1 d . . .
N2 N 0.2119(2) 0.18075(18) 0.77821(13) 0.0188(4) Uani 1 1 d . . .
C1 C -0.1055(3) 0.1072(2) 0.87229(17) 0.0213(5) Uani 1 1 d . . .
H1A H -0.2099 0.0498 0.8757 0.0599(19) Uiso 1 1 calc R . .
H1B H -0.1145 0.1900 0.8814 0.0599(19) Uiso 1 1 calc R . .
H1C H -0.0185 0.1021 0.9203 0.0599(19) Uiso 1 1 calc R . .
C2 C -0.0331(3) -0.2059(2) 0.72961(15) 0.0190(4) Uani 1 1 d . . .
C3 C -0.1628(3) -0.2740(2) 0.76572(17) 0.0214(5) Uani 1 1 d . . .
C4 C -0.2510(3) -0.3908(2) 0.71856(18) 0.0270(5) Uani 1 1 d . . .
H4 H -0.3392 -0.4369 0.7419 0.035(3) Uiso 1 1 calc R . .
C5 C -0.2138(3) -0.4411(2) 0.63903(19) 0.0305(6) Uani 1 1 d . . .
H5 H -0.2742 -0.5217 0.6088 0.035(3) Uiso 1 1 calc R . .
C6 C -0.0877(3) -0.3737(2) 0.60310(18) 0.0279(5) Uani 1 1 d . . .
H6 H -0.0626 -0.4091 0.5481 0.035(3) Uiso 1 1 calc R . .
C7 C 0.0030(3) -0.2553(2) 0.64586(17) 0.0226(5) Uani 1 1 d . . .
C8 C -0.2107(3) -0.2230(2) 0.85267(17) 0.0233(5) Uani 1 1 d . . .
H8 H -0.1264 -0.1435 0.8816 0.028(4) Uiso 1 1 calc R . .
C9 C -0.2179(3) -0.3084(3) 0.92245(19) 0.0332(6) Uani 1 1 d . . .
H9A H -0.3058 -0.3846 0.8970 0.0599(19) Uiso 1 1 calc R . .
H9B H -0.2398 -0.2693 0.9795 0.0599(19) Uiso 1 1 calc R . .
H9C H -0.1128 -0.3257 0.9353 0.0599(19) Uiso 1 1 calc R . .
C10 C -0.3773(3) -0.2002(3) 0.8294(2) 0.0345(6) Uani 1 1 d . . .
H10A H -0.3731 -0.1469 0.7840 0.0599(19) Uiso 1 1 calc R . .
H10B H -0.4030 -0.1613 0.8853 0.0599(19) Uiso 1 1 calc R . .
H10C H -0.4624 -0.2778 0.8038 0.0599(19) Uiso 1 1 calc R . .
C11 C 0.1342(3) -0.1804(2) 0.60205(17) 0.0256(5) Uani 1 1 d . . .
H11 H 0.1235 -0.0964 0.6085 0.028(4) Uiso 1 1 calc R . .
C12 C 0.1099(4) -0.2310(3) 0.4989(2) 0.0389(7) Uani 1 1 d . . .
H12A H 0.1844 -0.1735 0.4711 0.0599(19) Uiso 1 1 calc R . .
H12B H -0.0037 -0.2428 0.4692 0.0599(19) Uiso 1 1 calc R . .
H12C H 0.1336 -0.3091 0.4905 0.0599(19) Uiso 1 1 calc R . .
C13 C 0.3061(3) -0.1703(3) 0.6504(2) 0.0361(6) Uani 1 1 d . . .
H13A H 0.3245 -0.1295 0.7145 0.0599(19) Uiso 1 1 calc R . .
H13B H 0.3864 -0.1230 0.6194 0.0599(19) Uiso 1 1 calc R . .
H13C H 0.3185 -0.2518 0.6483 0.0599(19) Uiso 1 1 calc R . .
C14 C 0.1843(3) -0.0601(2) 0.84309(15) 0.0195(5) Uani 1 1 d . . .
C15 C 0.2176(3) -0.1648(2) 0.88438(18) 0.0260(5) Uani 1 1 d . . .
H15A H 0.1267 -0.2010 0.9135 0.0599(19) Uiso 1 1 calc R . .
H15B H 0.3197 -0.1347 0.9305 0.0599(19) Uiso 1 1 calc R . .
H15C H 0.2280 -0.2264 0.8358 0.0599(19) Uiso 1 1 calc R . .
C16 C 0.2951(3) 0.0557(2) 0.88002(16) 0.0222(5) Uani 1 1 d . . .
H16 H 0.3637 0.0625 0.9375 0.035(3) Uiso 1 1 calc R . .
C17 C 0.3192(3) 0.1632(2) 0.84407(16) 0.0213(5) Uani 1 1 d . . .
C18 C 0.4790(3) 0.2620(3) 0.88371(19) 0.0303(6) Uani 1 1 d . . .
H18A H 0.5265 0.2945 0.8337 0.0599(19) Uiso 1 1 calc R . .
H18B H 0.5555 0.2282 0.9186 0.0599(19) Uiso 1 1 calc R . .
H18C H 0.4588 0.3275 0.9246 0.0599(19) Uiso 1 1 calc R . .
C19 C 0.2542(3) 0.2842(2) 0.73348(16) 0.0204(5) Uani 1 1 d . . .
C20 C 0.2149(3) 0.3900(2) 0.76467(16) 0.0220(5) Uani 1 1 d . . .
C21 C 0.2455(3) 0.4844(2) 0.71464(18) 0.0273(5) Uani 1 1 d . . .
H21 H 0.2188 0.5566 0.7342 0.035(3) Uiso 1 1 calc R . .
C22 C 0.3136(3) 0.4740(2) 0.63767(19) 0.0312(6) Uani 1 1 d . . .
H22 H 0.3331 0.5386 0.6045 0.035(3) Uiso 1 1 calc R . .
C23 C 0.3537(3) 0.3696(2) 0.60850(18) 0.0297(6) Uani 1 1 d . . .
H23 H 0.4023 0.3638 0.5559 0.035(3) Uiso 1 1 calc R . .
C24 C 0.3238(3) 0.2726(2) 0.65508(17) 0.0236(5) Uani 1 1 d . . .
C25 C 0.1432(3) 0.4067(2) 0.84996(17) 0.0251(5) Uani 1 1 d . . .
H25 H 0.1334 0.3320 0.8773 0.028(4) Uiso 1 1 calc R . .
C26 C -0.0290(4) 0.4203(3) 0.8260(2) 0.0405(7) Uani 1 1 d . . .
H26A H -0.0217 0.4956 0.8023 0.0599(19) Uiso 1 1 calc R . .
H26B H -0.0768 0.4235 0.8813 0.0599(19) Uiso 1 1 calc R . .
H26C H -0.0985 0.3507 0.7791 0.0599(19) Uiso 1 1 calc R . .
C27 C 0.2549(4) 0.5156(3) 0.92200(19) 0.0356(6) Uani 1 1 d . . .
H27A H 0.3629 0.5039 0.9386 0.0599(19) Uiso 1 1 calc R . .
H27B H 0.2065 0.5227 0.9768 0.0599(19) Uiso 1 1 calc R . .
H27C H 0.2669 0.5900 0.8967 0.0599(19) Uiso 1 1 calc R . .
C28 C 0.3676(3) 0.1589(2) 0.61977(18) 0.0282(5) Uani 1 1 d . . .
H28 H 0.3158 0.0950 0.6535 0.028(4) Uiso 1 1 calc R . .
C29 C 0.5505(4) 0.1787(4) 0.6427(3) 0.0623(11) Uani 1 1 d . . .
H29A H 0.5736 0.1018 0.6242 0.0599(19) Uiso 1 1 calc R . .
H29B H 0.5902 0.2076 0.7090 0.0599(19) Uiso 1 1 calc R . .
H29C H 0.6061 0.2394 0.6097 0.0599(19) Uiso 1 1 calc R . .
C30 C 0.2994(6) 0.1098(4) 0.5198(2) 0.0645(11) Uani 1 1 d . . .
H30A H 0.3496 0.1688 0.4838 0.0599(19) Uiso 1 1 calc R . .
H30B H 0.1804 0.0954 0.5078 0.0599(19) Uiso 1 1 calc R . .
H30C H 0.3235 0.0332 0.5021 0.0599(19) 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'
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
_geom_angle_publ_flag
N1 Sn1 N2 84.69(7) . . ?
N1 Sn1 C1 92.95(8) . . ?
N2 Sn1 C1 92.69(9) . . ?
C14 N1 C2 120.78(18) . . ?
C14 N1 Sn1 122.26(16) . . ?
C2 N1 Sn1 116.44(13) . . ?
C17 N2 C19 121.3(2) . . ?
C17 N2 Sn1 123.21(16) . . ?
C19 N2 Sn1 115.44(14) . . ?
C3 C2 C7 120.3(2) . . ?
C3 C2 N1 120.8(2) . . ?
C7 C2 N1 118.8(2) . . ?
C4 C3 C2 118.6(2) . . ?
C4 C3 C8 119.2(2) . . ?
C2 C3 C8 122.2(2) . . ?
C5 C4 C3 121.6(2) . . ?
C4 C5 C6 119.8(3) . . ?
C5 C6 C7 121.4(2) . . ?
C6 C7 C2 118.2(2) . . ?
C6 C7 C11 120.5(2) . . ?
C2 C7 C11 121.3(2) . . ?
C3 C8 C10 110.1(2) . . ?
C3 C8 C9 111.9(2) . . ?
C10 C8 C9 109.6(2) . . ?
C13 C11 C7 112.1(2) . . ?
C13 C11 C12 110.1(2) . . ?
C7 C11 C12 111.9(2) . . ?
N1 C14 C16 124.4(2) . . ?
N1 C14 C15 119.2(2) . . ?
C16 C14 C15 116.4(2) . . ?
C14 C16 C17 129.3(2) . . ?
N2 C17 C16 123.9(2) . . ?
N2 C17 C18 119.6(2) . . ?
C16 C17 C18 116.5(2) . . ?
C20 C19 C24 121.3(2) . . ?
C20 C19 N2 119.9(2) . . ?
C24 C19 N2 118.6(2) . . ?
C19 C20 C21 118.1(2) . . ?
C19 C20 C25 122.7(2) . . ?
C21 C20 C25 119.2(2) . . ?
C22 C21 C20 121.1(2) . . ?
C21 C22 C23 120.1(2) . . ?
C22 C23 C24 121.0(2) . . ?
C23 C24 C19 118.4(2) . . ?
C23 C24 C28 119.3(2) . . ?
C19 C24 C28 122.4(2) . . ?
C20 C25 C27 111.5(2) . . ?
C20 C25 C26 111.0(2) . . ?
C27 C25 C26 110.4(2) . . ?
C30 C28 C29 111.7(3) . . ?
C30 C28 C24 113.1(3) . . ?
C29 C28 C24 111.5(2) . . ?
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
Sn1 N1 2.2091(18) . ?
Sn1 N2 2.218(2) . ?
Sn1 C1 2.253(2) . ?
N1 C14 1.331(3) . ?
N1 C2 1.438(3) . ?
N2 C17 1.327(3) . ?
N2 C19 1.447(3) . ?
C2 C3 1.413(3) . ?
C2 C7 1.420(3) . ?
C3 C4 1.390(4) . ?
C3 C8 1.516(3) . ?
C4 C5 1.374(4) . ?
C5 C6 1.386(4) . ?
C6 C7 1.392(4) . ?
C7 C11 1.524(3) . ?
C8 C10 1.533(3) . ?
C8 C9 1.537(3) . ?
C11 C13 1.518(4) . ?
C11 C12 1.537(4) . ?
C14 C16 1.404(4) . ?
C14 C15 1.517(3) . ?
C16 C17 1.407(3) . ?
C17 C18 1.511(3) . ?
C19 C20 1.402(3) . ?
C19 C24 1.404(3) . ?
C20 C21 1.404(3) . ?
C20 C25 1.512(3) . ?
C21 C22 1.376(4) . ?
C22 C23 1.383(4) . ?
C23 C24 1.395(4) . ?
C24 C28 1.520(4) . ?
C25 C27 1.531(4) . ?
C25 C26 1.534(4) . ?
C28 C30 1.494(4) . ?
C28 C29 1.512(4) . ?
