#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:58:16 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229228 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/65/7046551.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_7046551
loop_
_publ_author_name
'de Lima, G. M.'
'Walton, R. I.'
'Clarkson, G. J.'
'Bitzer, R. S.'
'Ardisson, J. D.'
_publ_section_title
;
 Air and moisture stable covalently-bonded tin(ii) coordination polymers.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8013
_journal_page_last               8022
_journal_paper_doi               10.1039/c8dt01370e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         '0.5(C10 H2 O8 Sn2)'
_chemical_formula_sum            'C5 H O4 Sn'
_chemical_formula_weight         243.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-02
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2018-03-14 deposited with the CCDC.
2018-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.645(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.85894(19)
_cell_length_b                   20.2345(5)
_cell_length_c                   4.51467(16)
_cell_measurement_reflns_used    2114
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.6080
_cell_measurement_theta_min      4.3570
_cell_volume                     520.12(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43d (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.1417
_diffrn_detector_type            Ruby
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -70.00  31.00   1.00   16.40    --  -41.71  57.00-150.00  101
  2  ω    -96.00   3.00   1.00   16.40    --  -41.71 125.00 -90.00   99
  3  ω   -115.00 -14.00   1.00   16.40    --  -41.71 -57.00  60.00  101
  4  ω     53.00 178.00   1.00   44.70    --  105.73  15.00  90.00  125
  5  ω     23.00 109.00   1.00   44.70    --  105.73 -95.00  90.00   86
  6  ω     33.00 132.00   1.00   44.70    --  105.73 -45.00 150.00   99
  7  ω     33.00 122.00   1.00   44.70    --  105.73-125.00  60.00   89
  8  ω     30.00 138.00   1.00   44.70    --  105.73 -77.00 150.00  108
  9  ω     77.00 178.00   1.00   44.70    --  105.73  30.00 150.00  101
 10  ω     23.00 109.00   1.00   44.70    --  105.73 -95.00 -30.00   86
 11  ω   -116.00 -17.00   1.00   16.40    --  -41.71 -38.00 -60.00   99
 12  ω   -115.00 -14.00   1.00   16.40    --  -41.71 -57.00 150.00  101
 13  ω   -115.00 -14.00   1.00   16.40    --  -41.71 -57.00-120.00  101
 14  ω     77.00 178.00   1.00   44.70    --  105.73  61.00 -30.00  101
 15  ω     77.00 178.00   1.00   44.70    --  105.73  61.00-180.00  101
 16  ω     73.00 178.00   1.00   44.70    --  105.73  77.00 -90.00  105
 17  ω     73.00 178.00   1.00   44.70    --  105.73  77.00-150.00  105
 18  ω     73.00 123.00   1.00   44.70    --  105.73  77.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1827009500
_diffrn_orient_matrix_UB_12      0.0551319500
_diffrn_orient_matrix_UB_13      -0.0079798000
_diffrn_orient_matrix_UB_21      0.1982988000
_diffrn_orient_matrix_UB_22      0.0517898000
_diffrn_orient_matrix_UB_23      0.0659944000
_diffrn_orient_matrix_UB_31      -0.0228309000
_diffrn_orient_matrix_UB_32      0.0086153000
_diffrn_orient_matrix_UB_33      -0.3447926000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       4
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2850
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.001
_diffrn_reflns_theta_min         4.370
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    38.657
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50441
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43d (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    3.113
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.927
_refine_diff_density_rms         0.176
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     48
_refine_ls_number_reflns         546
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0221
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0419P)²+0.6017P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0586
_refine_ls_wR_factor_ref         0.0587
_reflns_Friedel_coverage         0.000
_reflns_number_gt                540
_reflns_number_total             546
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01370e3.cif
_cod_data_source_block           gdl8
_cod_depositor_comments
'Adding full bibliography for 7046551--7046554.cif.'
_cod_database_code               7046551
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C20 H20 N2 O2 Sn'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C4(H4)
;
_shelx_res_file
;
TITL gdl8_a.res in C2/m
    gdl8.res
    created by SHELXL-2016/6 at 11:41:44 on 02-Mar-2017
REM Old TITL gdl8 in C2
REM SHELXT solution in C2/m
REM R1 0.093, Rweak 0.011, Alpha 0.022, Orientation as input
REM Formula found by SHELXT: C5 N2 O2 Sn
CELL 1.54184 5.858945 20.23448 4.514669 90 103.6451 90
ZERR 4 0.000187 0.000515 0.000156 0 0.0034 0
LATT 7
SYMM -X,+Y,-Z
SFAC C H O Sn
UNIT 20 4 16 4
EQIV $1 0.5-X,0.5-Y,2-Z
EQIV $2 1.5-X,0.5-Y,2-Z

L.S. 4 0 0
PLAN  20
TEMP 20(2)
RTAB dist Sn1 Sn1_$1
RTAB dist Sn1 Sn1_$2
BOND $H
list 4
fmap 2
acta
REM <olex2.extras>
REM <HklSrc "%./gdl8.hkl">
REM </olex2.extras>

WGHT    0.041900    0.601700
FVAR       2.54745
O1    3    0.698269    0.383681    0.877232    11.00000    0.03065    0.01412 =
         0.02174   -0.00460    0.01816   -0.00932
SN1   4    0.500000    0.302904    1.000000    10.50000    0.01557    0.00495 =
         0.02094    0.00000    0.01077    0.00000
C2    1    0.782783    0.378889    0.640767    11.00000    0.00956    0.00839 =
         0.01391    0.00032    0.00456   -0.00094
O2    3    0.757192    0.328774    0.474944    11.00000    0.01851    0.00734 =
         0.02052   -0.00367    0.00758   -0.00130
C3    1    0.906938    0.439970    0.572610    11.00000    0.01231    0.00699 =
         0.01294   -0.00153    0.00440   -0.00190
C4    1    0.817528    0.500000    0.643919    10.50000    0.01072    0.01008 =
         0.01466    0.00000    0.00625    0.00000
AFIX  43
H4    2    0.694612    0.500000    0.741953    10.50000   -1.20000
AFIX   0
HKLF 4




REM  gdl8_a.res in C2/m
REM R1 =  0.0221 for     540 Fo > 4sig(Fo)  and  0.0223 for all     546 data
REM     48 parameters refined using      0 restraints

END

WGHT      0.0419      0.6017

REM Highest difference peak  0.611,  deepest hole -0.927,  1-sigma level  0.176
Q1    1   0.7853  0.3427  1.0053  11.00000  0.05    0.61
Q2    1   0.2500  0.2500  1.0000  10.50000  0.05    0.52
Q3    1   0.2581  0.2408  0.8753  11.00000  0.05    0.52
Q4    1   0.3611  0.3073  0.9939  11.00000  0.05    0.48
Q5    1   0.8935  0.2882  0.8382  11.00000  0.05    0.48
Q6    1   0.7578  0.3615  0.1984  11.00000  0.05    0.45
Q7    1   0.7612  0.4433  1.0199  11.00000  0.05    0.44
Q8    1   0.8827  0.4102  0.6355  11.00000  0.05    0.42
Q9    1   0.7418  0.4267  0.2319  11.00000  0.05    0.40
Q10   1   0.4761  0.2606  0.6340  11.00000  0.05    0.38
Q11   1   0.4931  0.3619  0.6733  11.00000  0.05    0.37
Q12   1   1.0829  0.3901  0.7158  11.00000  0.05    0.37
Q13   1   0.6112  0.4289  0.3122  11.00000  0.05    0.37
Q14   1   0.5000  0.4030  0.5000  10.50000  0.05    0.33
Q15   1   0.5730  0.5000  0.7061  10.50000  0.05    0.31
Q16   1   0.4807  0.5000  0.6182  10.50000  0.05    0.30
Q17   1   0.4137  0.4845  0.6755  11.00000  0.05    0.29
Q18   1   1.0000  0.3272  1.0000  10.50000  0.05    0.29
Q19   1   0.7861  0.4082  0.4850  11.00000  0.05    0.27
Q20   1   0.5000  0.2304  1.0000  10.50000  0.05    0.26
;
_shelx_res_checksum              28437
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.672
_oxdiff_exptl_absorpt_empirical_full_min 0.754
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
O1 O 0.6983(5) 0.38368(12) 0.8772(6) 0.0202(6) Uani 1 1 d . . .
Sn1 Sn 0.500000 0.30290(2) 1.000000 0.01274(17) Uani 1 2 d S T P
C2 C 0.7828(5) 0.37889(15) 0.6408(7) 0.0103(6) Uani 1 1 d . . .
O2 O 0.7572(4) 0.32877(11) 0.4749(6) 0.0150(5) Uani 1 1 d . . .
C3 C 0.9069(6) 0.43997(15) 0.5726(7) 0.0105(6) Uani 1 1 d . . .
C4 C 0.8175(8) 0.500000 0.6439(10) 0.0113(8) Uani 1 2 d S T P
H4 H 0.694612 0.500000 0.741953 0.014 Uiso 1 2 calc RS T P
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0307(14) 0.0141(12) 0.0217(13) -0.0046(10) 0.0182(11) -0.0093(10)
Sn1 0.0156(2) 0.0049(2) 0.0209(2) 0.000 0.01077(15) 0.000
C2 0.0096(14) 0.0084(15) 0.0139(15) 0.0003(12) 0.0046(11) -0.0009(11)
O2 0.0185(12) 0.0073(11) 0.0205(12) -0.0037(9) 0.0076(9) -0.0013(9)
C3 0.0123(15) 0.0070(14) 0.0129(14) -0.0015(11) 0.0044(13) -0.0019(12)
C4 0.011(2) 0.010(2) 0.015(2) 0.000 0.0063(16) 0.000
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sn Sn 0.0259 5.4591 '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
C2 O1 Sn1 119.7(2) . .
O1 Sn1 O1 81.17(13) . 2_657
O1 Sn1 O2 78.38(9) 2_657 2_656
O1 Sn1 O2 82.29(9) 2_657 1_556
O1 Sn1 O2 78.38(9) . 1_556
O1 Sn1 O2 82.29(9) . 2_656
O2 Sn1 O2 154.48(11) 1_556 2_656
O1 C2 C3 114.1(3) . .
O2 C2 O1 123.1(3) . .
O2 C2 C3 122.7(3) . .
C2 O2 Sn1 133.1(2) . 1_554
C3 C3 C2 124.38(17) 2_756 .
C4 C3 C2 116.4(3) . .
C4 C3 C3 119.1(2) . 2_756
C3 C4 C3 121.8(4) 6_565 .
C3 C4 H4 119.1 6_565 .
C3 C4 H4 119.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 Sn1 2.152(2) .
O1 C2 1.282(4) .
Sn1 O2 2.370(3) 2_656
Sn1 O2 2.370(3) 1_556
C2 O2 1.248(4) .
C2 C3 1.502(4) .
C3 C3 1.399(6) 2_756
C3 C4 1.390(4) .
C4 H4 0.9300 .
