#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/07/7010731.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_7010731
loop_
_publ_author_name
'Harrison, William T. A.'
'Howie, R. Alan'
'Munro, Craig M.'
'Wardell, James L.'
_publ_section_title
;
 Monomer--polymer forms of solid, unsolvated, 5-coordinate
 halodimethyl(2-diphenylphosphinylethyl)stannanes, XMe2SnCH2CH2P(O)Ph2
 (X = Cl, Br or I). Effects of different
 recrystallisation media
;
_journal_issue                   18
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2593
_journal_paper_doi               10.1039/b103107b
_journal_year                    2001
_chemical_formula_moiety         'C16 H20 Cl O P Sn'
_chemical_formula_sum            'C16 H20 Cl O P Sn'
_chemical_formula_weight         413.43
_chemical_name_systematic
; 
Chlorodimethyl(2-diphenylphosphinoethyl-C,O)stannane 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 109.9570(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7708(4)
_cell_length_b                   15.1394(6)
_cell_length_c                   12.6876(5)
_cell_measurement_reflns_used    10432
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      1.71
_cell_volume                     1764.10(12)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  SHEXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD'
_diffrn_measurement_method       'φ and ω'
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0149
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            10432
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.684
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.702
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS: Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.557
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             824
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3104
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0242
_refine_ls_R_factor_gt           0.0195
_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)+(0.0285P)²+0.4754P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0499
_refine_ls_wR_factor_ref         0.0520
_reflns_number_gt                2717
_reflns_number_total             3104
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b103107b.txt
_cod_data_source_block           clmrt
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_database_code               7010731
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, z'
'-x, -y, -z'
'-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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.102281(16) 0.055216(10) 0.217437(13) 0.04682(7) Uani 1 d . . .
Cl1 Cl 0.24883(8) 0.13729(6) 0.12054(7) 0.0804(2) Uani 1 d . . .
P1 P -0.21046(6) 0.02903(4) 0.25908(5) 0.04619(14) Uani 1 d . . .
O1 O -0.05905(16) -0.00987(12) 0.30184(13) 0.0523(4) Uani 1 d . . .
C1 C 0.2567(3) 0.06726(19) 0.3817(2) 0.0641(7) Uani 1 d . . .
H1A H 0.2070 0.0677 0.4352 0.096 Uiso 1 calc R . .
H1B H 0.3100 0.1213 0.3875 0.096 Uiso 1 calc R . .
H1C H 0.3228 0.0182 0.3968 0.096 Uiso 1 calc R . .
C2 C 0.0951(3) -0.06753(17) 0.1357(2) 0.0617(7) Uani 1 d . . .
H2A H 0.1695 -0.0690 0.1022 0.093 Uiso 1 calc R . .
H2B H 0.0015 -0.0747 0.0786 0.093 Uiso 1 calc R . .
H2C H 0.1110 -0.1145 0.1893 0.093 Uiso 1 calc R . .
C3 C -0.0839(3) 0.14090(16) 0.1526(2) 0.0556(6) Uani 1 d . . .
H3A H -0.0744 0.1896 0.2043 0.067 Uiso 1 calc R . .
H3B H -0.0853 0.1653 0.0815 0.067 Uiso 1 calc R . .
C4 C -0.2273(3) 0.09339(18) 0.1354(2) 0.0559(6) Uani 1 d . . .
H4A H -0.2505 0.0550 0.0705 0.067 Uiso 1 calc R . .
H4B H -0.3053 0.1361 0.1225 0.067 Uiso 1 calc R . .
C5 C -0.2405(2) 0.10189(15) 0.36100(19) 0.0467(5) Uani 1 d . . .
C6 C -0.3704(3) 0.14886(18) 0.3387(2) 0.0606(6) Uani 1 d . . .
H6 H -0.4446 0.1425 0.2699 0.073 Uiso 1 calc R . .
C7 C -0.3883(3) 0.20469(19) 0.4188(3) 0.0711(8) Uani 1 d . . .
H7 H -0.4752 0.2355 0.4044 0.085 Uiso 1 calc R . .
C8 C -0.2767(4) 0.21496(19) 0.5210(3) 0.0708(8) Uani 1 d . . .
H8 H -0.2884 0.2536 0.5743 0.085 Uiso 1 calc R . .
C9 C -0.1493(3) 0.16837(19) 0.5438(2) 0.0658(7) Uani 1 d . . .
H9 H -0.0754 0.1747 0.6128 0.079 Uiso 1 calc R . .
C10 C -0.1314(3) 0.11217(17) 0.4641(2) 0.0544(6) Uani 1 d . . .
H10 H -0.0450 0.0807 0.4796 0.065 Uiso 1 calc R . .
C11 C -0.3479(3) -0.05575(16) 0.2252(2) 0.0505(6) Uani 1 d . . .
C12 C -0.3653(3) -0.1093(2) 0.1322(3) 0.0696(7) Uani 1 d . . .
H12 H -0.3108 -0.0986 0.0860 0.083 Uiso 1 calc R . .
C13 C -0.4641(4) -0.1786(2) 0.1087(3) 0.0854(10) Uani 1 d . . .
H13 H -0.4749 -0.2146 0.0471 0.102 Uiso 1 calc R . .
C14 C -0.5452(3) -0.1942(2) 0.1750(3) 0.0858(10) Uani 1 d . . .
H14 H -0.6118 -0.2405 0.1581 0.103 Uiso 1 calc R . .
C15 C -0.5291(3) -0.1421(2) 0.2660(3) 0.0777(9) Uani 1 d . . .
H15 H -0.5850 -0.1531 0.3111 0.093 Uiso 1 calc R . .
C16 C -0.4306(3) -0.07309(18) 0.2922(2) 0.0611(7) Uani 1 d . . .
H16 H -0.4198 -0.0383 0.3549 0.073 Uiso 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'
Cl Cl 0.1484 0.1585 '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'
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
C2 Sn1 C1 116.73(11) . . ?
C2 Sn1 C3 117.30(10) . . ?
C1 Sn1 C3 123.18(10) . . ?
C2 Sn1 O1 86.62(9) . . ?
C1 Sn1 O1 87.25(9) . . ?
C3 Sn1 O1 79.63(7) . . ?
C2 Sn1 Cl1 97.10(8) . . ?
C1 Sn1 Cl1 96.04(8) . . ?
C3 Sn1 Cl1 93.63(7) . . ?
O1 Sn1 Cl1 173.24(4) . . ?
O1 P1 C5 111.17(10) . . ?
O1 P1 C11 111.54(11) . . ?
C5 P1 C11 108.51(11) . . ?
O1 P1 C4 108.07(10) . . ?
C5 P1 C4 107.74(12) . . ?
C11 P1 C4 109.73(12) . . ?
P1 O1 Sn1 113.06(9) . . ?
C4 C3 Sn1 112.69(16) . . ?
C3 C4 P1 108.90(16) . . ?
C10 C5 C6 119.2(2) . . ?
C10 C5 P1 119.06(18) . . ?
C6 C5 P1 121.78(19) . . ?
C7 C6 C5 119.9(3) . . ?
C6 C7 C8 120.0(3) . . ?
C9 C8 C7 120.4(3) . . ?
C8 C9 C10 119.7(3) . . ?
C9 C10 C5 120.9(2) . . ?
C16 C11 C12 118.9(3) . . ?
C16 C11 P1 122.20(19) . . ?
C12 C11 P1 118.8(2) . . ?
C13 C12 C11 119.7(3) . . ?
C14 C13 C12 120.6(3) . . ?
C13 C14 C15 120.0(3) . . ?
C14 C15 C16 120.7(3) . . ?
C11 C16 C15 120.1(3) . . ?
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 C2 2.117(2) . ?
Sn1 C1 2.123(3) . ?
Sn1 C3 2.156(2) . ?
Sn1 O1 2.3989(15) . ?
Sn1 Cl1 2.5114(7) . ?
P1 O1 1.5107(16) . ?
P1 C5 1.798(2) . ?
P1 C11 1.801(3) . ?
P1 C4 1.806(2) . ?
C3 C4 1.523(3) . ?
C5 C10 1.386(3) . ?
C5 C6 1.397(3) . ?
C6 C7 1.378(4) . ?
C7 C8 1.390(4) . ?
C8 C9 1.373(4) . ?
C9 C10 1.378(4) . ?
C11 C16 1.383(4) . ?
C11 C12 1.393(4) . ?
C12 C13 1.388(4) . ?
C13 C14 1.358(5) . ?
C14 C15 1.363(5) . ?
C15 C16 1.383(4) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 P1 O1 Sn1 -104.93(11) . . . . ?
C11 P1 O1 Sn1 133.82(11) . . . . ?
C4 P1 O1 Sn1 13.12(14) . . . . ?
C2 Sn1 O1 P1 -110.70(12) . . . . ?
C1 Sn1 O1 P1 132.30(12) . . . . ?
C3 Sn1 O1 P1 7.84(11) . . . . ?
C2 Sn1 C3 C4 49.1(2) . . . . ?
C1 Sn1 C3 C4 -111.30(19) . . . . ?
O1 Sn1 C3 C4 -31.55(17) . . . . ?
Cl1 Sn1 C3 C4 149.05(17) . . . . ?
Sn1 C3 C4 P1 46.9(2) . . . . ?
O1 P1 C4 C3 -38.1(2) . . . . ?
C5 P1 C4 C3 82.16(19) . . . . ?
C11 P1 C4 C3 -159.88(17) . . . . ?
O1 P1 C5 C10 -2.4(2) . . . . ?
C11 P1 C5 C10 120.64(19) . . . . ?
C4 P1 C5 C10 -120.61(19) . . . . ?
O1 P1 C5 C6 177.12(19) . . . . ?
C11 P1 C5 C6 -59.9(2) . . . . ?
C4 P1 C5 C6 58.9(2) . . . . ?
C10 C5 C6 C7 0.1(4) . . . . ?
P1 C5 C6 C7 -179.3(2) . . . . ?
C5 C6 C7 C8 0.7(4) . . . . ?
C6 C7 C8 C9 -1.3(4) . . . . ?
C7 C8 C9 C10 1.0(4) . . . . ?
C8 C9 C10 C5 -0.1(4) . . . . ?
C6 C5 C10 C9 -0.5(4) . . . . ?
P1 C5 C10 C9 179.03(19) . . . . ?
O1 P1 C11 C16 105.9(2) . . . . ?
C5 P1 C11 C16 -16.9(2) . . . . ?
C4 P1 C11 C16 -134.4(2) . . . . ?
O1 P1 C11 C12 -70.0(2) . . . . ?
C5 P1 C11 C12 167.2(2) . . . . ?
C4 P1 C11 C12 49.7(2) . . . . ?
C16 C11 C12 C13 -0.1(4) . . . . ?
P1 C11 C12 C13 175.9(2) . . . . ?
C11 C12 C13 C14 0.7(5) . . . . ?
C12 C13 C14 C15 -0.6(5) . . . . ?
C13 C14 C15 C16 0.0(5) . . . . ?
C12 C11 C16 C15 -0.5(4) . . . . ?
P1 C11 C16 C15 -176.4(2) . . . . ?
C14 C15 C16 C11 0.6(4) . . . . ?
