#------------------------------------------------------------------------------
#$Date: 2019-03-05 10:52:05 +0200 (Tue, 05 Mar 2019) $
#$Revision: 213973 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/01/07/7010738.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_7010738
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 I O P Sn'
_chemical_formula_sum            'C16 H20 I O P Sn'
_chemical_formula_weight         504.88
_chemical_name_systematic
; 
Catena[iododimethyl(2-diphenylphosphinoethyl)stannane]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7840(4)
_cell_length_b                   11.9471(5)
_cell_length_c                   14.2380(6)
_cell_measurement_reflns_used    7413
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      44.9
_cell_measurement_theta_min      2.5
_cell_volume                     1834.39(13)
_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  SHELXL-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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0263
_diffrn_reflns_av_sigmaI/netI    0.0217
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            11013
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.23
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.157
_exptl_absorpt_correction_T_max  0.8619
_exptl_absorpt_correction_T_min  0.6127
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS: Bruker, 1999)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_refine_diff_density_max         0.660
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         3222
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.014
_refine_ls_R_factor_all          0.0202
_refine_ls_R_factor_gt           0.0185
_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)+(0.0258P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0430
_refine_ls_wR_factor_ref         0.0436
_reflns_number_gt                3080
_reflns_number_total             3222
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b103107b.txt
_cod_data_source_block           iprt
_cod_database_code               7010738
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.159883(19) 0.151497(19) -0.093229(16) 0.03631(7) Uani 1 d . . .
I1 I 0.12256(3) -0.02802(3) -0.23616(2) 0.06157(10) Uani 1 d . . .
P1 P -0.28192(8) 0.12557(7) -0.08688(7) 0.0379(2) Uani 1 d . . .
O1 O -0.3255(3) 0.2138(2) -0.0199(2) 0.0570(7) Uani 1 d . . .
C1 C 0.3002(4) 0.0583(4) -0.0229(3) 0.0660(13) Uani 1 d . . .
H1A H 0.3791 0.0937 -0.0324 0.099 Uiso 1 calc R . .
H1B H 0.3027 -0.0164 -0.0478 0.099 Uiso 1 calc R . .
H1C H 0.2820 0.0554 0.0430 0.099 Uiso 1 calc R . .
C2 C 0.2083(5) 0.2720(4) -0.1954(3) 0.0684(14) Uani 1 d . . .
H2A H 0.2479 0.3344 -0.1654 0.103 Uiso 1 calc R . .
H2B H 0.1349 0.2970 -0.2272 0.103 Uiso 1 calc R . .
H2C H 0.2643 0.2391 -0.2401 0.103 Uiso 1 calc R . .
C3 C -0.0287(3) 0.1375(3) -0.0479(3) 0.0451(9) Uani 1 d . . .
H3A H -0.0395 0.0656 -0.0171 0.054 Uiso 1 calc R . .
H3B H -0.0447 0.1952 -0.0015 0.054 Uiso 1 calc R . .
C4 C -0.1251(3) 0.1477(3) -0.1264(2) 0.0421(8) Uani 1 d . . .
H4A H -0.1061 0.0935 -0.1750 0.050 Uiso 1 calc R . .
H4B H -0.1191 0.2217 -0.1541 0.050 Uiso 1 calc R . .
C5 C -0.3759(3) 0.1240(3) -0.1912(3) 0.0418(8) Uani 1 d . . .
C6 C -0.3964(5) 0.2224(4) -0.2392(4) 0.0735(13) Uani 1 d . . .
H6 H -0.3635 0.2892 -0.2166 0.088 Uiso 1 calc R . .
C7 C -0.4665(6) 0.2220(5) -0.3214(4) 0.0869(17) Uani 1 d . . .
H7 H -0.4800 0.2886 -0.3535 0.104 Uiso 1 calc R . .
C8 C -0.5145(5) 0.1264(5) -0.3545(4) 0.0766(15) Uani 1 d . . .
H8 H -0.5610 0.1273 -0.4094 0.092 Uiso 1 calc R . .
C9 C -0.4960(7) 0.0295(6) -0.3089(4) 0.101(2) Uani 1 d . . .
H9 H -0.5298 -0.0367 -0.3318 0.121 Uiso 1 calc R . .
C10 C -0.4265(5) 0.0293(4) -0.2281(4) 0.0803(15) Uani 1 d . . .
H10 H -0.4134 -0.0384 -0.1973 0.096 Uiso 1 calc R . .
C11 C -0.2885(3) -0.0113(3) -0.0348(2) 0.0397(8) Uani 1 d . . .
C12 C -0.2184(4) -0.0999(3) -0.0689(3) 0.0522(10) Uani 1 d . . .
H12 H -0.1643 -0.0890 -0.1189 0.063 Uiso 1 calc R . .
C13 C -0.2296(5) -0.2043(4) -0.0280(4) 0.0679(13) Uani 1 d . . .
H13 H -0.1821 -0.2634 -0.0507 0.081 Uiso 1 calc R . .
C14 C -0.3090(5) -0.2223(4) 0.0451(3) 0.0699(13) Uani 1 d . . .
H14 H -0.3149 -0.2929 0.0724 0.084 Uiso 1 calc R . .
C15 C -0.3802(5) -0.1351(4) 0.0782(3) 0.0697(13) Uani 1 d . . .
H15 H -0.4353 -0.1475 0.1274 0.084 Uiso 1 calc R . .
C16 C -0.3708(4) -0.0308(4) 0.0397(3) 0.0539(10) Uani 1 d . . .
H16 H -0.4191 0.0275 0.0630 0.065 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'
I I -0.4742 1.8119 '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 120.3(2) . . ?
C2 Sn1 C3 119.76(18) . . ?
C1 Sn1 C3 119.50(18) . . ?
C2 Sn1 O1 89.34(16) . 3 ?
C1 Sn1 O1 89.32(15) . 3 ?
C3 Sn1 O1 84.72(12) . 3 ?
C2 Sn1 I1 93.06(14) . . ?
C1 Sn1 I1 92.31(13) . . ?
C3 Sn1 I1 91.23(10) . . ?
O1 Sn1 I1 175.92(8) 3 . ?
O1 P1 C11 111.44(17) . . ?
O1 P1 C5 110.89(16) . . ?
C11 P1 C5 108.00(16) . . ?
O1 P1 C4 112.97(18) . . ?
C11 P1 C4 107.42(17) . . ?
C5 P1 C4 105.81(17) . . ?
P1 O1 Sn1 165.40(19) . 3_455 ?
C4 C3 Sn1 114.7(2) . . ?
C3 C4 P1 113.4(3) . . ?
C10 C5 C6 117.0(4) . . ?
C10 C5 P1 123.6(3) . . ?
C6 C5 P1 119.4(3) . . ?
C5 C6 C7 120.0(5) . . ?
C8 C7 C6 120.6(5) . . ?
C7 C8 C9 120.6(5) . . ?
C8 C9 C10 119.1(5) . . ?
C5 C10 C9 122.7(5) . . ?
C12 C11 C16 118.8(4) . . ?
C12 C11 P1 121.9(3) . . ?
C16 C11 P1 119.2(3) . . ?
C13 C12 C11 119.6(4) . . ?
C14 C13 C12 121.2(5) . . ?
C13 C14 C15 119.4(4) . . ?
C16 C15 C14 120.8(4) . . ?
C15 C16 C11 120.1(4) . . ?
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 2.112(4) . ?
Sn1 C1 2.129(4) . ?
Sn1 C3 2.141(3) . ?
Sn1 O1 2.282(3) 3 ?
Sn1 I1 2.9838(4) . ?
P1 O1 1.497(3) . ?
P1 C11 1.796(4) . ?
P1 C5 1.799(4) . ?
P1 C4 1.801(3) . ?
O1 Sn1 2.282(3) 3_455 ?
C3 C4 1.532(5) . ?
C5 C10 1.362(6) . ?
C5 C6 1.378(6) . ?
C6 C7 1.393(7) . ?
C7 C8 1.339(8) . ?
C8 C9 1.343(8) . ?
C9 C10 1.373(7) . ?
C11 C12 1.388(5) . ?
C11 C16 1.403(5) . ?
C12 C13 1.382(6) . ?
C13 C14 1.365(7) . ?
C14 C15 1.377(7) . ?
C15 C16 1.366(6) . ?
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
C11 P1 O1 Sn1 88.5(8) . . . 3_455 ?
C5 P1 O1 Sn1 -151.1(8) . . . 3_455 ?
C4 P1 O1 Sn1 -32.5(8) . . . 3_455 ?
C2 Sn1 C3 C4 40.8(3) . . . . ?
C1 Sn1 C3 C4 -146.8(3) . . . . ?
O1 Sn1 C3 C4 127.0(3) 3 . . . ?
I1 Sn1 C3 C4 -53.4(3) . . . . ?
Sn1 C3 C4 P1 175.84(19) . . . . ?
O1 P1 C4 C3 65.5(3) . . . . ?
C11 P1 C4 C3 -57.9(3) . . . . ?
C5 P1 C4 C3 -173.0(3) . . . . ?
O1 P1 C5 C10 -130.8(4) . . . . ?
C11 P1 C5 C10 -8.4(4) . . . . ?
C4 P1 C5 C10 106.4(4) . . . . ?
O1 P1 C5 C6 51.1(4) . . . . ?
C11 P1 C5 C6 173.5(3) . . . . ?
C4 P1 C5 C6 -71.7(4) . . . . ?
C10 C5 C6 C7 0.2(7) . . . . ?
P1 C5 C6 C7 178.4(4) . . . . ?
C5 C6 C7 C8 0.1(9) . . . . ?
C6 C7 C8 C9 0.0(9) . . . . ?
C7 C8 C9 C10 -0.4(10) . . . . ?
C6 C5 C10 C9 -0.5(9) . . . . ?
P1 C5 C10 C9 -178.7(5) . . . . ?
C8 C9 C10 C5 0.7(11) . . . . ?
O1 P1 C11 C12 -158.9(3) . . . . ?
C5 P1 C11 C12 79.1(3) . . . . ?
C4 P1 C11 C12 -34.6(4) . . . . ?
O1 P1 C11 C16 24.0(3) . . . . ?
C5 P1 C11 C16 -98.0(3) . . . . ?
C4 P1 C11 C16 148.3(3) . . . . ?
C16 C11 C12 C13 -1.0(6) . . . . ?
P1 C11 C12 C13 -178.1(3) . . . . ?
C11 C12 C13 C14 0.4(7) . . . . ?
C12 C13 C14 C15 0.7(7) . . . . ?
C13 C14 C15 C16 -1.0(7) . . . . ?
C14 C15 C16 C11 0.4(7) . . . . ?
C12 C11 C16 C15 0.7(6) . . . . ?
P1 C11 C16 C15 177.8(3) . . . . ?
