#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/10/48/7104855.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_7104855
loop_
_publ_author_name
'Driess, Matthias'
'Merz, Klaus'
'Monsé, Christian'
_publ_section_title
;
 Synthesis of the first fluoro(phosphanyl)- and diphosphanyl-stannanes
 and surprising formation of [P(SnMe3)4]+SiF5-
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   20
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2608
_journal_page_last               2609
_journal_paper_doi               10.1039/b308660g
_journal_year                    2003
_chemical_formula_sum            'C30 H50 P2 Sn'
_chemical_formula_weight         591.33
_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                105.176(17)
_cell_angle_beta                 96.941(15)
_cell_angle_gamma                93.621(13)
_cell_formula_units_Z            2
_cell_length_a                   9.8122(18)
_cell_length_b                   10.394(2)
_cell_length_c                   16.662(4)
_cell_measurement_reflns_used    36
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      16.2
_cell_measurement_theta_min      3.5
_cell_volume                     1620.1(6)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1996)'
_computing_publication_material  'SHELXTL (Siemens, 1996)'
_computing_structure_refinement  'SHELXTL (Siemens, 1996)'
_computing_structure_solution    'SHELXTL (Siemens, 1996)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.754
_diffrn_measured_fraction_theta_max 0.686
_diffrn_measurement_device_type  'Bruker axs CCD 1000'
_diffrn_measurement_method       omega-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    0.0201
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            3999
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         25.17
_diffrn_reflns_theta_min         2.04
_exptl_absorpt_coefficient_mu    0.902
_exptl_absorpt_correction_T_max  0.7342
_exptl_absorpt_correction_T_min  0.6549
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             620
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.046
_refine_diff_density_min         -1.171
_refine_diff_density_rms         0.160
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         3999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0519
_refine_ls_R_factor_gt           0.0458
_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)+(0.1222P)²+0.5072P] where
P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1423
_refine_ls_wR_factor_ref         0.1594
_reflns_number_gt                3609
_reflns_number_total             3999
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b308660g.txt
_cod_data_source_block           p-1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7104855
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 0.96351(5) 0.98255(3) 0.251334(19) 0.0260(3) Uani 1 1 d . . .
C1 C 0.8752(7) 0.8729(5) 0.3300(3) 0.0243(16) Uani 1 1 d . . .
P2 P 0.9085(3) 1.22099(15) 0.26352(12) 0.0526(7) Uani 1 1 d . . .
C16 C 0.8734(10) 0.8671(5) 0.1245(3) 0.030(2) Uani 1 1 d . . .
C3 C 0.8324(8) 0.6560(5) 0.3573(3) 0.0306(18) Uani 1 1 d . . .
H3A H 0.8479 0.5651 0.3462 0.037 Uiso 1 1 calc R . .
P1 P 1.2210(3) 1.0084(2) 0.29648(12) 0.0518(7) Uani 1 1 d . . .
C5 C 0.7284(7) 0.8424(5) 0.4308(3) 0.0287(16) Uani 1 1 d . . .
H5A H 0.6721 0.8785 0.4713 0.034 Uiso 1 1 calc R . .
C6 C 0.7882(7) 0.9262(5) 0.3908(3) 0.0292(17) Uani 1 1 d . . .
C17 C 0.9543(9) 0.8003(5) 0.0618(3) 0.025(2) Uani 1 1 d . . .
C2 C 0.8978(7) 0.7362(5) 0.3147(3) 0.0296(17) Uani 1 1 d . . .
C19 C 0.7387(11) 0.7007(6) -0.0301(4) 0.030(2) Uani 1 1 d . . .
C18 C 0.8767(12) 0.7182(5) -0.0132(3) 0.036(3) Uani 1 1 d . . .
H18A H 0.9261 0.6719 -0.0547 0.044 Uiso 1 1 calc R . .
C20 C 0.6637(9) 0.7672(6) 0.0321(3) 0.0329(19) Uani 1 1 d . . .
H20A H 0.5668 0.7561 0.0224 0.039 Uiso 1 1 calc R . .
C28 C 0.6397(8) 0.9182(7) 0.1709(4) 0.041(2) Uani 1 1 d . . .
H28A H 0.7014 0.9706 0.2221 0.049 Uiso 1 1 calc R . .
C4 C 0.7468(8) 0.7056(6) 0.4147(3) 0.0364(19) Uani 1 1 d . . .
C21 C 0.7315(11) 0.8493(6) 0.1077(4) 0.035(2) Uani 1 1 d . . .
C10 C 0.6750(8) 0.6155(6) 0.4583(4) 0.039(2) Uani 1 1 d . . .
H10A H 0.6215 0.6710 0.4986 0.047 Uiso 1 1 calc R . .
C13 C 0.7649(8) 1.0738(5) 0.4131(3) 0.0317(18) Uani 1 1 d . . .
H13A H 0.7620 1.1022 0.3607 0.038 Uiso 1 1 calc R . .
C8 C 1.1128(10) 0.6167(7) 0.2952(4) 0.057(2) Uani 1 1 d . . .
H8A H 1.1703 0.5752 0.2542 0.086 Uiso 1 1 calc R . .
H8B H 1.0782 0.5510 0.3216 0.086 Uiso 1 1 calc R . .
H8C H 1.1668 0.6903 0.3375 0.086 Uiso 1 1 calc R . .
C25 C 0.6704(9) 0.6123(6) -0.1152(4) 0.042(2) Uani 1 1 d . . .
H25A H 0.7170 0.5290 -0.1270 0.050 Uiso 1 1 calc R . .
C22 C 1.1070(10) 0.8206(6) 0.0744(3) 0.031(2) Uani 1 1 d . . .
H22A H 1.1376 0.8330 0.1350 0.038 Uiso 1 1 calc R . .
C15 C 0.8913(10) 1.1540(6) 0.4738(5) 0.056(3) Uani 1 1 d . . .
H15A H 0.8778 1.2486 0.4886 0.085 Uiso 1 1 calc R . .
H15B H 0.9734 1.1405 0.4468 0.085 Uiso 1 1 calc R . .
H15C H 0.9021 1.1235 0.5243 0.085 Uiso 1 1 calc R . .
C7 C 0.9933(8) 0.6687(5) 0.2519(3) 0.0335(18) Uani 1 1 d . . .
H7A H 1.0317 0.7381 0.2276 0.040 Uiso 1 1 calc R . .
C26 C 0.6919(9) 0.6794(7) -0.1837(4) 0.052(2) Uani 1 1 d . . .
H26A H 0.7897 0.7040 -0.1813 0.079 Uiso 1 1 calc R . .
H26B H 0.6433 0.7593 -0.1756 0.079 Uiso 1 1 calc R . .
H26C H 0.6565 0.6181 -0.2380 0.079 Uiso 1 1 calc R . .
C14 C 0.6350(11) 1.1077(8) 0.4474(6) 0.065(3) Uani 1 1 d . . .
H14A H 0.5571 1.0562 0.4082 0.098 Uiso 1 1 calc R . .
H14B H 0.6264 1.2026 0.4555 0.098 Uiso 1 1 calc R . .
H14C H 0.6366 1.0864 0.5008 0.098 Uiso 1 1 calc R . .
C9 C 0.9099(9) 0.5594(6) 0.1797(4) 0.051(2) Uani 1 1 d . . .
H9A H 0.9707 0.5180 0.1409 0.076 Uiso 1 1 calc R . .
H9B H 0.8393 0.5987 0.1505 0.076 Uiso 1 1 calc R . .
H9C H 0.8666 0.4922 0.2019 0.076 Uiso 1 1 calc R . .
C11 C 0.5752(12) 0.5092(9) 0.3946(6) 0.085(4) Uani 1 1 d . . .
H11A H 0.5094 0.5521 0.3646 0.127 Uiso 1 1 calc R . .
H11B H 0.5265 0.4549 0.4235 0.127 Uiso 1 1 calc R . .
H11C H 0.6260 0.4527 0.3551 0.127 Uiso 1 1 calc R . .
C30 C 0.5443(10) 0.8153(9) 0.1974(5) 0.069(3) Uani 1 1 d . . .
H30A H 0.4881 0.8630 0.2373 0.103 Uiso 1 1 calc R . .
H30B H 0.6005 0.7594 0.2232 0.103 Uiso 1 1 calc R . .
H30C H 0.4849 0.7596 0.1482 0.103 Uiso 1 1 calc R . .
C27 C 0.5139(11) 0.5715(9) -0.1173(5) 0.070(3) Uani 1 1 d . . .
H27A H 0.4759 0.5155 -0.1729 0.105 Uiso 1 1 calc R . .
H27B H 0.4657 0.6514 -0.1044 0.105 Uiso 1 1 calc R . .
H27C H 0.5029 0.5222 -0.0761 0.105 Uiso 1 1 calc R . .
C23 C 1.1558(10) 0.9480(9) 0.0551(6) 0.064(3) Uani 1 1 d . . .
H23A H 1.1093 1.0213 0.0853 0.097 Uiso 1 1 calc R . .
H23B H 1.1350 0.9376 -0.0048 0.097 Uiso 1 1 calc R . .
H23C H 1.2547 0.9673 0.0724 0.097 Uiso 1 1 calc R . .
C12 C 0.7830(10) 0.5520(9) 0.5082(6) 0.065(3) Uani 1 1 d . . .
H12A H 0.8450 0.6224 0.5483 0.098 Uiso 1 1 calc R . .
H12B H 0.8354 0.4958 0.4696 0.098 Uiso 1 1 calc R . .
H12C H 0.7360 0.4981 0.5380 0.098 Uiso 1 1 calc R . .
C29 C 0.5590(11) 1.0177(9) 0.1358(5) 0.072(3) Uani 1 1 d . . .
H29A H 0.6228 1.0792 0.1203 0.107 Uiso 1 1 calc R . .
H29B H 0.5085 1.0677 0.1782 0.107 Uiso 1 1 calc R . .
H29C H 0.4948 0.9693 0.0867 0.107 Uiso 1 1 calc R . .
C24 C 1.1807(12) 0.7036(9) 0.0267(6) 0.074(3) Uani 1 1 d . . .
H24A H 1.1490 0.6218 0.0393 0.111 Uiso 1 1 calc R . .
H24B H 1.2795 0.7226 0.0440 0.111 Uiso 1 1 calc R . .
H24C H 1.1600 0.6929 -0.0333 0.111 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'
P P 0.1023 0.0942 '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
C1 Sn1 C16 103.0(2) . . ?
C1 Sn1 P1 105.93(18) . . ?
C16 Sn1 P1 120.8(2) . . ?
C1 Sn1 P2 119.20(15) . . ?
C16 Sn1 P2 105.85(16) . . ?
P1 Sn1 P2 103.09(8) . . ?
C2 C1 C6 118.3(5) . . ?
C2 C1 Sn1 116.8(4) . . ?
C6 C1 Sn1 124.7(4) . . ?
C21 C16 C17 119.7(6) . . ?
C21 C16 Sn1 116.7(4) . . ?
C17 C16 Sn1 123.4(6) . . ?
C4 C3 C2 122.2(5) . . ?
C6 C5 C4 123.5(6) . . ?
C5 C6 C1 118.8(5) . . ?
C5 C6 C13 120.2(5) . . ?
C1 C6 C13 121.0(5) . . ?
C18 C17 C16 115.0(8) . . ?
C18 C17 C22 122.7(6) . . ?
C16 C17 C22 122.3(6) . . ?
C3 C2 C1 119.9(5) . . ?
C3 C2 C7 117.4(5) . . ?
C1 C2 C7 122.8(5) . . ?
C18 C19 C20 117.7(6) . . ?
C18 C19 C25 119.3(6) . . ?
C20 C19 C25 123.0(9) . . ?
C19 C18 C17 125.6(6) . . ?
C21 C20 C19 120.5(8) . . ?
C29 C28 C21 109.7(6) . . ?
C29 C28 C30 112.7(8) . . ?
C21 C28 C30 112.2(6) . . ?
C3 C4 C5 117.2(5) . . ?
C3 C4 C10 121.0(5) . . ?
C5 C4 C10 121.8(6) . . ?
C16 C21 C20 121.4(6) . . ?
C16 C21 C28 122.4(6) . . ?
C20 C21 C28 116.2(8) . . ?
C4 C10 C11 110.1(6) . . ?
C4 C10 C12 110.3(7) . . ?
C11 C10 C12 111.6(7) . . ?
C14 C13 C6 115.8(6) . . ?
C14 C13 C15 110.9(6) . . ?
C6 C13 C15 108.6(6) . . ?
C26 C25 C19 110.5(6) . . ?
C26 C25 C27 110.8(6) . . ?
C19 C25 C27 113.0(6) . . ?
C17 C22 C23 110.7(6) . . ?
C17 C22 C24 116.0(6) . . ?
C23 C22 C24 109.8(8) . . ?
C8 C7 C9 112.2(5) . . ?
C8 C7 C2 111.6(5) . . ?
C9 C7 C2 110.3(6) . . ?
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 C1 2.167(5) . ?
Sn1 C16 2.186(6) . ?
Sn1 P1 2.524(3) . ?
Sn1 P2 2.5311(17) . ?
C1 C2 1.413(7) . ?
C1 C6 1.427(8) . ?
C16 C21 1.378(11) . ?
C16 C17 1.446(9) . ?
C3 C4 1.369(9) . ?
C3 C2 1.401(8) . ?
C5 C6 1.373(8) . ?
C5 C4 1.404(8) . ?
C6 C13 1.521(7) . ?
C17 C18 1.414(10) . ?
C17 C22 1.482(11) . ?
C2 C7 1.550(8) . ?
C19 C18 1.340(11) . ?
C19 C20 1.402(9) . ?
C19 C25 1.522(9) . ?
C20 C21 1.386(9) . ?
C28 C29 1.532(11) . ?
C28 C21 1.533(10) . ?
C28 C30 1.561(11) . ?
C4 C10 1.516(8) . ?
C10 C11 1.518(11) . ?
C10 C12 1.553(12) . ?
C13 C14 1.485(11) . ?
C13 C15 1.543(11) . ?
C8 C7 1.506(10) . ?
C25 C26 1.513(9) . ?
C25 C27 1.561(13) . ?
C22 C23 1.506(10) . ?
C22 C24 1.542(10) . ?
C7 C9 1.529(9) . ?
