#------------------------------------------------------------------------------
#$Date: 2016-03-24 01:58:58 +0200 (Thu, 24 Mar 2016) $
#$Revision: 179549 $
#$URL: svn://www.crystallography.net/cod/cif/4/50/18/4501866.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_4501866
loop_
_publ_author_name
'Wang, Xiqu'
'Liu, Lumei'
'Makarenko, Tatyana'
'Jacobson, Allan J.'
_publ_section_title
;
 Influence of Ligand Geometry on the Dimensionality of Sn(II)
 Benzenedicarboxylate Crystal Structures
;
_journal_issue                   8
_journal_name_full               'Crystal Growth & Design'
_journal_page_first              3752
_journal_paper_doi               10.1021/cg1005874
_journal_volume                  10
_journal_year                    2010
_chemical_formula_sum            'C16 H8 O9 Sn3'
_chemical_formula_weight         700.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.7610(10)
_cell_angle_beta                 89.700(2)
_cell_angle_gamma                64.0700(10)
_cell_formula_units_Z            2
_cell_length_a                   6.9475(10)
_cell_length_b                   7.1514(11)
_cell_length_c                   19.140(3)
_cell_measurement_reflns_used    6227
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      28.01
_cell_measurement_theta_min      3.19
_cell_volume                     849.2(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.963
_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  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            6537
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.99
_diffrn_reflns_theta_min         3.19
_exptl_absorpt_coefficient_mu    4.430
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.608
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.200
_refine_ls_extinction_coef       0.0026(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         3568
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_gt           0.0338
_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/[σ²(Fo²)+(0.0645P)²+1.4304P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1007
_refine_ls_wR_factor_ref         0.1017
_reflns_number_gt                3426
_reflns_number_total             3568
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg1005874_si_005.cif
_cod_data_source_block           Sn3O(1,4-bdc)2
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4501866
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
C1 C 0.3011(7) 0.4064(7) 0.1152(2) 0.0245(9) Uani 1 1 d .
C2 C 0.1451(7) 0.4535(6) 0.0557(2) 0.0230(8) Uani 1 1 d .
C3 C 0.1763(8) 0.5407(7) -0.0100(2) 0.0253(9) Uani 1 1 d .
H3 H 0.2963 0.5680 -0.0164 0.030 Uiso 1 1 calc R
C4 C 0.0311(7) 0.5862(7) -0.0650(2) 0.0255(9) Uani 1 1 d .
H4 H 0.0517 0.6446 -0.1092 0.031 Uiso 1 1 calc R
C5 C 0.3758(7) 0.0424(7) 0.3532(2) 0.0239(8) Uani 1 1 d .
C6 C 0.4433(6) 0.0189(7) 0.4290(2) 0.0206(8) Uani 1 1 d .
C7 C 0.5089(7) -0.1726(7) 0.4708(2) 0.0218(8) Uani 1 1 d .
H7 H 0.5157 -0.2896 0.4509 0.026 Uiso 1 1 calc R
C8 C -0.0432(7) -0.2089(7) 0.3856(2) 0.0240(8) Uani 1 1 d .
C9 C -0.0227(7) -0.0989(7) 0.4444(2) 0.0228(8) Uani 1 1 d .
C10 C 0.0466(7) -0.2117(7) 0.5107(2) 0.0258(9) Uani 1 1 d .
H10 H 0.0769 -0.3542 0.5177 0.031 Uiso 1 1 calc R
C11 C 0.0709(7) -0.1129(7) 0.5665(2) 0.0257(9) Uani 1 1 d .
H11 H 0.1196 -0.1888 0.6112 0.031 Uiso 1 1 calc R
C12 C 0.6194(7) -0.1414(6) 0.1481(2) 0.0227(8) Uani 1 1 d .
C13 C 0.5557(7) -0.0679(6) 0.0714(2) 0.0205(8) Uani 1 1 d .
C14 C 0.6783(7) 0.0085(6) 0.0301(2) 0.0229(8) Uani 1 1 d .
H14 H 0.7985 0.0141 0.0503 0.027 Uiso 1 1 calc R
C15 C 0.5638(7) -0.1917(7) 0.5412(2) 0.0247(9) Uani 1 1 d .
H15 H 0.6061 -0.3210 0.5692 0.030 Uiso 1 1 calc R
C16 C 0.6213(7) 0.0764(7) -0.0413(2) 0.0236(8) Uani 1 1 d .
H16 H 0.7034 0.1282 -0.0691 0.028 Uiso 1 1 calc R
O1 O -0.1221(5) -0.1072(5) 0.32473(17) 0.0285(7) Uani 1 1 d .
O2 O 0.0214(6) -0.4028(5) 0.39448(19) 0.0349(8) Uani 1 1 d .
O3 O 0.7908(6) -0.1500(6) 0.17176(18) 0.0354(8) Uani 1 1 d .
O4 O 0.3605(6) -0.1112(5) 0.33029(18) 0.0316(7) Uani 1 1 d .
O5 O 0.3331(6) 0.2139(5) 0.31621(17) 0.0295(7) Uani 1 1 d .
O6 O 0.2877(6) 0.2992(5) 0.17179(17) 0.0275(7) Uani 1 1 d .
O7 O 0.4408(6) 0.4748(6) 0.11227(18) 0.0334(7) Uani 1 1 d .
O8 O 0.5010(5) -0.2014(5) 0.18642(17) 0.0274(7) Uani 1 1 d .
O9 O 0.2245(5) -0.3657(4) 0.25021(16) 0.0223(6) Uani 1 1 d .
Sn1 Sn 0.18164(5) -0.05645(4) 0.230858(15) 0.02195(13) Uani 1 1 d .
Sn2 Sn -0.05105(5) -0.40647(5) 0.273214(16) 0.02456(13) Uani 1 1 d .
Sn3 Sn 0.50521(5) 0.36930(4) 0.238572(17) 0.02577(13) Uani 1 1 d .
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'
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
O7 C1 O6 119.8(4) . .
O7 C1 C2 121.6(4) . .
O6 C1 C2 118.6(4) . .
C4 C2 C3 120.1(4) 2_565 .
C4 C2 C1 120.3(4) 2_565 .
C3 C2 C1 119.7(4) . .
C4 C3 C2 119.7(4) . .
C3 C4 C2 120.2(4) . 2_565
O5 C5 O4 123.8(4) . .
O5 C5 C6 118.4(4) . .
O4 C5 C6 117.8(4) . .
C7 C6 C15 119.4(4) . 2_656
C7 C6 C5 120.8(4) . .
C15 C6 C5 119.8(4) 2_656 .
C15 C7 C6 120.6(4) . .
O2 C8 O1 119.5(4) . .
O2 C8 C9 119.8(4) . .
O1 C8 C9 120.7(4) . .
C10 C9 C11 120.6(4) . 2_556
C10 C9 C8 118.7(4) . .
C11 C9 C8 120.7(4) 2_556 .
C9 C10 C11 119.8(4) . .
C9 C11 C10 119.6(4) 2_556 .
O3 C12 O8 121.9(4) . .
O3 C12 C13 119.1(4) . .
O8 C12 C13 118.9(4) . .
C16 C13 C14 119.9(4) 2_655 .
C16 C13 C12 121.0(4) 2_655 .
C14 C13 C12 119.1(4) . .
C16 C14 C13 119.7(4) . .
C7 C15 C6 120.0(4) . 2_656
C13 C16 C14 120.5(4) 2_655 .
C8 O1 Sn2 93.5(3) . .
C8 O2 Sn2 91.1(3) . .
C12 O3 Sn2 114.0(3) . 1_655
C5 O4 Sn1 118.6(3) . .
C5 O5 Sn3 139.3(3) . .
C1 O6 Sn3 95.8(3) . .
C1 O7 Sn3 87.2(3) . .
C12 O8 Sn1 137.4(3) . .
Sn3 O9 Sn1 125.83(15) 1_545 .
Sn3 O9 Sn2 117.68(13) 1_545 .
Sn1 O9 Sn2 116.16(14) . .
O9 Sn1 O4 87.24(13) . .
O9 Sn1 O8 83.50(12) . .
O4 Sn1 O8 84.76(13) . .
O9 Sn2 O1 79.12(12) . .
O9 Sn2 O2 88.51(13) . .
O1 Sn2 O2 55.67(11) . .
O9 Sn2 O3 84.17(12) . 1_455
O1 Sn2 O3 80.98(13) . 1_455
O2 Sn2 O3 136.63(13) . 1_455
O9 Sn3 O6 82.25(12) 1_565 .
O9 Sn3 O5 80.93(11) 1_565 .
O6 Sn3 O5 73.25(12) . .
O9 Sn3 O7 86.66(12) 1_565 .
O6 Sn3 O7 56.08(12) . .
O5 Sn3 O7 129.01(12) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 O7 1.262(6) .
C1 O6 1.284(5) .
C1 C2 1.482(7) .
C2 C4 1.379(6) 2_565
C2 C3 1.401(6) .
C3 C4 1.372(7) .
C4 C2 1.379(6) 2_565
C5 O5 1.261(6) .
C5 O4 1.272(6) .
C5 C6 1.495(6) .
C6 C7 1.394(6) .
C6 C15 1.398(6) 2_656
C7 C15 1.378(6) .
C8 O2 1.248(6) .
C8 O1 1.289(6) .
C8 C9 1.483(6) .
C9 C10 1.391(6) .
C9 C11 1.392(6) 2_556
C10 C11 1.393(7) .
C11 C9 1.392(6) 2_556
C12 O3 1.250(6) .
C12 O8 1.278(5) .
C12 C13 1.503(6) .
C13 C16 1.390(7) 2_655
C13 C14 1.398(6) .
C14 C16 1.398(6) .
C15 C6 1.398(6) 2_656
C16 C13 1.390(7) 2_655
O1 Sn2 2.308(3) .
O2 Sn2 2.383(4) .
O3 Sn2 2.414(3) 1_655
O4 Sn1 2.181(3) .
O5 Sn3 2.378(3) .
O6 Sn3 2.234(3) .
O7 Sn3 2.436(3) .
O8 Sn1 2.209(3) .
O9 Sn3 2.074(3) 1_545
O9 Sn1 2.089(3) .
O9 Sn2 2.096(3) .
Sn2 O3 2.414(3) 1_455
Sn3 O9 2.074(3) 1_565
