#------------------------------------------------------------------------------
#$Date: 2016-02-19 16:29:56 +0200 (Fri, 19 Feb 2016) $
#$Revision: 176759 $
#$URL: svn://www.crystallography.net/cod/cif/2/00/92/2009282.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2009282
loop_
_publ_author_name
'Lu, Zaisheng'
'Burgess, John'
'Fawcett, John'
'Russell, David R.'
_publ_section_title
;
 Bis(2-ethyl-3-hydroxy-4-pyranonato)diiodotin(IV) acetonitrile solvate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2051
_journal_page_last               2053
_journal_paper_doi               10.1107/S0108270199011683
_journal_volume                  55
_journal_year                    1999
_chemical_formula_iupac          '[Sn I2 (C7 H7 O3)2], C2 H3 N'
_chemical_formula_moiety         'C14 H14 I2 O6 Sn, C2 H3 N'
_chemical_formula_sum            'C16 H17 I2 N O6 Sn'
_chemical_formula_weight         691.80
_chemical_name_systematic
;
Bis-(2-ethyl-3-Hydroxy-pyranonato)diiodotin(IV) acetonitrile
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           SHELXTL/PC
_cell_angle_alpha                90.00
_cell_angle_beta                 95.170(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.6580(10)
_cell_length_b                   25.364(4)
_cell_length_c                   11.500(2)
_cell_measurement_reflns_used    37
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.47
_cell_measurement_theta_min      5.30
_cell_volume                     2224.6(6)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Fait, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXTL/PC
_computing_structure_refinement  SHELXTL/PC
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1996)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       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  0.031
_diffrn_reflns_av_sigmaI/netI    0.0572
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.79
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.952
_exptl_absorpt_correction_T_max  0.647
_exptl_absorpt_correction_T_min  0.181
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details
;
For the absorption correction, 530 ψ-scan data were measured and the
correction was applied using XEMP [in SHELXTL/PC (Sheldrick, 1996) based
on North et al. (1968)]; R = 0.048 before and 0.031 after correction.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.59
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3911
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.077
_refine_ls_R_factor_gt           0.044
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0313P)²+1.5444P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.098
_reflns_number_gt                2730
_reflns_number_total             3911
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ha1269.cif
_cod_data_source_block           9556
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2009282
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Sn1 0.17894(7) 0.119870(19) 0.80755(4) 0.05075(15) Uani d . 1 . . Sn
I1 -0.12783(8) 0.16619(2) 0.85988(5) 0.0756(2) Uani d . 1 . . I
I2 0.06278(9) 0.08808(3) 0.58729(5) 0.0830(2) Uani d . 1 . . I
O1 0.4055(7) 0.07759(19) 0.7959(5) 0.0660(14) Uani d . 1 . . O
O2 0.1176(7) 0.04899(19) 0.8939(4) 0.0604(13) Uani d . 1 . . O
O3 0.4964(8) -0.0580(2) 0.8644(5) 0.0752(16) Uani d . 1 . . O
C1 0.690(3) -0.0231(6) 0.6654(17) 0.263(14) Uani d . 1 . . C
H1A 0.8041 -0.0169 0.6399 0.394 Uiso calc R 1 . . H
H1B 0.6023 -0.0089 0.6090 0.394 Uiso calc R 1 . . H
H1C 0.6716 -0.0603 0.6733 0.394 Uiso calc R 1 . . H
C2 0.6784(12) 0.0003(4) 0.7677(9) 0.093(3) Uani d . 1 . . C
H2A 0.6928 0.0379 0.7572 0.111 Uiso calc R 1 . . H
H2B 0.7758 -0.0117 0.8209 0.111 Uiso calc R 1 . . H
C3 0.5174(11) -0.0082(3) 0.8233(7) 0.069(2) Uani d . 1 . . C
C4 0.3890(10) 0.0276(3) 0.8342(6) 0.0519(18) Uani d . 1 . . C
C5 0.2359(9) 0.0141(3) 0.8871(6) 0.0486(17) Uani d . 1 . . C
C6 0.2211(11) -0.0386(3) 0.9275(7) 0.060(2) Uani d . 1 . . C
H6A 0.1227 -0.0496 0.9627 0.072 Uiso calc R 1 . . H
C7 0.3505(14) -0.0710(3) 0.9134(8) 0.078(3) Uani d . 1 . . C
H7A 0.3402 -0.1055 0.9393 0.093 Uiso calc R 1 . . H
O1A 0.3042(6) 0.18752(17) 0.7589(4) 0.0491(11) Uani d . 1 . . O
O2A 0.2953(7) 0.1462(2) 0.9725(4) 0.0602(13) Uani d . 1 . . O
O3A 0.5666(8) 0.2800(2) 0.9310(5) 0.0802(17) Uani d . 1 . . O
C1A 0.558(2) 0.3395(4) 0.7303(10) 0.144(6) Uani d . 1 . . C
H1AA 0.5716 0.3516 0.6525 0.215 Uiso calc R 1 . . H
H1AB 0.6680 0.3426 0.7770 0.215 Uiso calc R 1 . . H
H1AC 0.4715 0.3606 0.7639 0.215 Uiso calc R 1 . . H
C2A 0.5025(15) 0.2849(3) 0.7266(8) 0.091(3) Uani d . 1 . . C
H2AA 0.5872 0.2651 0.6862 0.109 Uiso calc R 1 . . H
H2AB 0.3917 0.2831 0.6787 0.109 Uiso calc R 1 . . H
C3A 0.4796(11) 0.2570(3) 0.8372(6) 0.061(2) Uani d . 1 . . C
C4A 0.3874(9) 0.2117(3) 0.8494(6) 0.0470(17) Uani d . 1 . . C
C5A 0.3810(10) 0.1891(3) 0.9624(6) 0.0527(18) Uani d . 1 . . C
C6A 0.4730(11) 0.2157(3) 1.0573(7) 0.067(2) Uani d . 1 . . C
H6AA 0.4724 0.2027 1.1329 0.080 Uiso calc R 1 . . H
C7A 0.5602(13) 0.2594(4) 1.0367(8) 0.080(3) Uani d . 1 . . C
H7AA 0.6200 0.2766 1.0997 0.096 Uiso calc R 1 . . H
C8 0.5618(17) 0.1483(6) 0.5414(10) 0.149(5) Uani d . 1 . . C
H8A 0.6541 0.1658 0.5885 0.224 Uiso calc R 1 . . H
H8B 0.5686 0.1110 0.5558 0.224 Uiso calc R 1 . . H
H8C 0.4504 0.1613 0.5608 0.224 Uiso calc R 1 . . H
C9 0.5799(15) 0.1580(5) 0.4239(10) 0.106(4) Uani d . 1 . . C
N1 0.601(2) 0.1632(6) 0.3304(11) 0.189(6) Uani d . 1 . . N
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'
O O 0.0106 0.0060 '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'
I I -0.4742 1.8119 '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_publ_flag
O1 Sn1 O1A 90.03(19) y
O1 Sn1 O2 79.20(19) y
O1A Sn1 O2 162.81(19) y
O1 Sn1 O2A 86.2(2) y
O1A Sn1 O2A 79.25(18) y
O2 Sn1 O2A 86.6(2) y
O1 Sn1 I2 89.54(16) y
O1A Sn1 I2 96.58(12) y
O2 Sn1 I2 96.68(15) y
O2A Sn1 I2 174.02(15) y
O1 Sn1 I1 169.56(15) y
O1A Sn1 I1 97.55(13) y
O2 Sn1 I1 91.71(14) y
O2A Sn1 I1 88.17(14) y
I2 Sn1 I1 96.67(3) y
C4 O1 Sn1 111.4(4) ?
C5 O2 Sn1 111.7(4) ?
C7 O3 C3 120.3(6) ?
C1 C2 C3 116.8(11) ?
C4 C3 O3 118.7(7) ?
C4 C3 C2 126.4(8) ?
O3 C3 C2 114.9(7) ?
O1 C4 C3 120.7(7) ?
O1 C4 C5 118.3(6) ?
C3 C4 C5 121.0(7) ?
O2 C5 C4 118.8(6) ?
O2 C5 C6 123.6(7) ?
C4 C5 C6 117.6(7) ?
C7 C6 C5 117.8(7) ?
C6 C7 O3 124.5(7) ?
C4A O1A Sn1 112.0(4) ?
C5A O2A Sn1 111.2(4) ?
C7A O3A C3A 120.5(7) ?
C1A C2A C3A 119.2(8) ?
O3A C3A C4A 120.3(7) ?
O3A C3A C2A 113.2(7) ?
C4A C3A C2A 126.5(7) ?
O1A C4A C3A 121.9(6) ?
O1A C4A C5A 118.5(7) ?
C3A C4A C5A 119.6(7) ?
O2A C5A C6A 124.0(7) ?
O2A C5A C4A 119.0(7) ?
C6A C5A C4A 117.1(7) ?
C7A C6A C5A 119.0(8) ?
C6A C7A O3A 123.5(8) ?
N1 C9 C8 175.8(18) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Sn1 O1 . 2.054(5) y
Sn1 O1A . 2.067(4) y
Sn1 O2 . 2.127(5) y
Sn1 O2A . 2.130(5) y
Sn1 I2 . 2.7298(9) y
Sn1 I1 . 2.7417(8) y
O1 C4 . 1.351(8) y
O2 C5 . 1.274(8) y
O3 C7 . 1.338(11) ?
O3 C3 . 1.362(9) ?
C1 C2 . 1.327(16) ?
C2 C3 . 1.455(11) ?
C3 C4 . 1.353(10) ?
C4 C5 . 1.411(10) y
C5 C6 . 1.422(10) ?
C6 C7 . 1.309(11) ?
O1A C4A . 1.321(8) y
O2A C5A . 1.281(9) y
O3A C7A . 1.327(10) ?
O3A C3A . 1.348(9) ?
C1A C2A . 1.449(12) ?
C2A C3A . 1.480(11) ?
C3A C4A . 1.363(10) ?
C4A C5A . 1.426(9) y
C5A C6A . 1.416(10) ?
C6A C7A . 1.327(12) ?
C8 C9 . 1.392(15) ?
C9 N1 . 1.109(14) ?
