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#$Date: 2016-03-24 00:54:54 +0100 (Thu, 24 Mar 2016) $
#$Revision: 179546 $
#$URL: svn://saulius.grazulis.lt/cod-secondary/cif/4/50/15/4501518.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_4501518
loop_
_publ_author_name
'Wang, Xiqu'
'Liu, Lumei'
'Makarenko, Tatyana'
'Jacobson, Allan J.'
_publ_section_title
;
 Acentric and Centric Interpenetrations of an Anionic Framework Mediated
 by Cation Sizes: The Alkali-Metal Tin(II) Benzenedicarboxylates
 A2Sn2(bdc)3(H2O)x(A = Li, Na, K, Rb, Cs)
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1960
_journal_paper_doi               10.1021/cg100049s
_journal_volume                  10
_journal_year                    2010
_chemical_formula_sum            'C24 H16 Li2 O14 Sn2'
_chemical_formula_weight         779.63
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           197
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                   13.7784(2)
_cell_length_b                   13.7784(2)
_cell_length_c                   13.7784(2)
_cell_measurement_reflns_used    7534
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.85
_cell_measurement_theta_min      2.96
_cell_volume                     2615.75(7)
_computing_cell_refinement       Bruker-ApexII
_computing_data_collection       Bruker-ApexII
_computing_data_reduction        Bruker-ApexII
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    Bruker-ApexII
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  Bruker-ApexII
_diffrn_measurement_method       'narrow frame'
_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  0.0459
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8306
_diffrn_reflns_theta_full        29.03
_diffrn_reflns_theta_max         29.03
_diffrn_reflns_theta_min         2.09
_exptl_absorpt_coefficient_mu    1.983
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.822
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.980
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1512
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.206
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.047
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_coef       0.00086(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1116
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.092
_refine_ls_R_factor_all          0.0146
_refine_ls_R_factor_gt           0.0145
_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/[\s^2^(Fo^2^)+(0.0234P)^2^+0.8108P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0386
_refine_ls_wR_factor_ref         0.0387
_reflns_number_gt                1108
_reflns_number_total             1116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg100049s_si_002.cif
_cod_data_source_block           Li2Sn2(bdc)3(H2O)2
_cod_original_sg_symbol_H-M      I23
_cod_database_code               4501518
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'z+1/2, x+1/2, y+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x+1/2'
'-y+1/2, -z+1/2, x+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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Sn1 Sn 0.600016(7) 0.399984(7) 0.600016(7) 0.02824(8) Uani 1 3 d S
O1 O 0.75728(9) 0.39461(11) 0.61599(11) 0.0386(3) Uani 1 1 d .
O2 O 0.73810(11) 0.55197(11) 0.63003(14) 0.0491(4) Uani 1 1 d .
C2 C 0.89950(13) 0.49021(13) 0.63175(11) 0.0305(3) Uani 1 1 d .
C1 C 0.79105(13) 0.48046(13) 0.62631(12) 0.0318(4) Uani 1 1 d .
C3 C 0.94112(16) 0.58124(15) 0.6331(2) 0.0493(6) Uani 1 1 d .
H3 H 0.9019 0.6362 0.6343 0.059 Uiso 1 1 calc R
C4 C 0.95851(15) 0.40900(15) 0.6328(2) 0.0479(5) Uani 1 1 d .
H4 H 0.9308 0.3474 0.6333 0.058 Uiso 1 1 calc R
O3W O 0.74207(14) 0.74207(14) 0.74207(14) 0.0763(10) Uani 1 3 d SD
Li1 Li 0.6649(2) 0.6649(2) 0.6649(2) 0.0335(11) Uani 1 3 d S
H1 H 0.730(7) 0.726(7) 0.797(2) 0.050 Uiso 0.33333 1 d PD
H2 H 0.783(9) 0.785(9) 0.745(4) 0.050 Uiso 0.33333 1 d PD
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
Sn1 0.02824(8) 0.02824(8) 0.02824(8) 0.00370(4) -0.00370(4) 0.00370(4)
O1 0.0280(6) 0.0353(6) 0.0524(8) 0.0056(7) -0.0006(5) -0.0019(5)
O2 0.0327(7) 0.0387(8) 0.0757(11) -0.0058(7) 0.0037(7) 0.0070(6)
C2 0.0283(7) 0.0321(8) 0.0311(7) 0.0009(6) 0.0023(6) 0.0002(7)
C1 0.0287(8) 0.0375(9) 0.0292(7) 0.0024(6) 0.0033(6) 0.0000(7)
C3 0.0308(9) 0.0317(10) 0.0852(17) -0.0002(9) 0.0053(9) 0.0041(7)
C4 0.0336(9) 0.0260(9) 0.0842(16) 0.0026(10) -0.0059(9) -0.0029(8)
O3W 0.0763(10) 0.0763(10) 0.0763(10) -0.0250(9) -0.0250(9) -0.0250(9)
Li1 0.0335(11) 0.0335(11) 0.0335(11) -0.0019(12) -0.0019(12) -0.0019(12)
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'
O O 0.0106 0.0060 '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'
Li Li -0.0003 0.0001 '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'
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
O1 Sn1 O1 82.09(6) . 12_665
O1 Sn1 O1 82.09(6) . 6_566
O1 Sn1 O1 82.09(6) 12_665 6_566
C1 O1 Sn1 109.97(12) . .
C1 O2 Li1 167.4(2) . .
C3 C2 C4 119.41(17) . .
C3 C2 C1 119.71(17) . .
C4 C2 C1 120.86(16) . .
O2 C1 O1 122.07(18) . .
O2 C1 C2 121.17(17) . .
O1 C1 C2 116.75(16) . .
C2 C3 C4 120.12(19) . 2_765
C2 C3 H3 119.9 . .
C4 C3 H3 119.9 2_765 .
C2 C4 C3 120.45(19) . 2_765
C2 C4 H4 119.8 . .
C3 C4 H4 119.8 2_765 .
Li1 O3W H1 105(4) . .
Li1 O3W H2 148(4) . .
H1 O3W H2 107(3) . .
O3W Li1 O2 108.04(16) . 5
O3W Li1 O2 108.04(16) . .
O2 Li1 O2 110.86(16) 5 .
O3W Li1 O2 108.04(16) . 9
O2 Li1 O2 110.86(16) 5 9
O2 Li1 O2 110.86(16) . 9
O3W Li1 H1 20.8(9) . .
O2 Li1 H1 125(2) 5 .
O2 Li1 H1 108(3) . .
O2 Li1 H1 89.4(16) 9 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sn1 O1 2.1793(13) .
Sn1 O1 2.1793(13) 12_665
Sn1 O1 2.1793(13) 6_566
O1 C1 1.279(2) .
O2 C1 1.227(2) .
O2 Li1 1.915(2) .
C2 C3 1.379(3) .
C2 C4 1.383(3) .
C2 C1 1.502(3) .
C3 C4 1.389(3) 2_765
C3 H3 0.9300 .
C4 C3 1.389(3) 2_765
C4 H4 0.9300 .
O3W Li1 1.842(6) .
O3W H1 0.80(2) .
O3W H2 0.81(2) .
Li1 O2 1.915(2) 5
Li1 O2 1.915(2) 9
Li1 H1 2.19(5) .
