#------------------------------------------------------------------------------
#$Date: 2016-03-22 12:51:35 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178966 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/95/4119582.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_4119582
loop_
_publ_author_name
'Richard F. D'Vries'
'Victor A. de la Peña-O'Shea'
'Natalia Snejko'
'Marta Iglesias'
'Enrique Gutiérrez-Puebla'
'M. Angeles Monge'
_publ_contact_author
;
        M.A. Monge Bravo
        Instituto de Ciencia de Materiales
        CSIC
        Campus de Cantoblanco
        28049 MADRID
        Spain
;
_publ_contact_author_email       amonge@icmm.csic.es
_publ_contact_author_fax         '34 1 372-0623'
_publ_contact_author_phone       '34 1 334-9025'
_publ_section_title
;
 H3O2 Bridging Ligand in a Metal-Organic Framework. Insight into the
 Aqua-Hydroxo←\\rightarrowHydroxyl Equilibrium: A Combined
 Experimental and Theoretical Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5782
_journal_page_last               5792
_journal_paper_doi               10.1021/ja4005046
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         'C14 H15 O22 S4 Sc3'
_chemical_formula_sum            'C14 H15 O22 S4 Sc3'
_chemical_formula_weight         798.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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                100.366(3)
_cell_angle_beta                 99.102(3)
_cell_angle_gamma                104.809(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5624(5)
_cell_length_b                   9.2132(6)
_cell_length_c                   9.7011(6)
_cell_measurement_reflns_used    4621
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      63.54
_cell_measurement_theta_min      4.74
_cell_volume                     627.81(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0120
_diffrn_reflns_av_sigmaI/netI    0.0182
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            2739
_diffrn_reflns_theta_full        63.70
_diffrn_reflns_theta_max         63.70
_diffrn_reflns_theta_min         4.74
_exptl_absorpt_coefficient_mu    10.885
_exptl_absorpt_correction_T_max  0.2275
_exptl_absorpt_correction_T_min  0.1018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_description       prism
_exptl_crystal_F_000             402
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.343
_refine_diff_density_min         -0.392
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0252
_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)+(0.0432P)²+0.5935P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0721
_reflns_number_gt                1880
_reflns_number_total             1949
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4005046_si_002.cif
_cod_data_source_block           data2t
_cod_database_code               4119582
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
Sc2 Sc 0.5000 0.5000 0.5000 0.01541(17) Uani 1 2 d S
Sc1 Sc 0.55117(6) 0.88948(5) 0.73907(4) 0.01552(15) Uani 1 1 d .
C1 C 0.3463(3) 0.3938(3) 1.1635(2) 0.0168(5) Uani 1 1 d .
C2 C 0.2744(3) 0.4472(3) 1.0350(2) 0.0163(5) Uani 1 1 d .
C3 C 0.2654(3) 0.5983(3) 1.0502(3) 0.0174(5) Uani 1 1 d .
H3 H 0.302(4) 0.665(3) 1.140(3) 0.015(6) Uiso 1 1 d .
C4 C 0.2058(3) 0.6463(3) 0.9275(3) 0.0155(5) Uani 1 1 d .
C5 C 0.1517(3) 0.5474(3) 0.7924(3) 0.0173(5) Uani 1 1 d .
H5 H 0.115(4) 0.587(3) 0.713(4) 0.032(8) Uiso 1 1 d .
C6 C 0.1650(3) 0.3987(3) 0.7802(2) 0.0158(5) Uani 1 1 d .
C7 C 0.2262(3) 0.3475(3) 0.8998(3) 0.0180(5) Uani 1 1 d .
H7 H 0.233(4) 0.244(4) 0.886(3) 0.028(8) Uiso 1 1 d .
O7 O 0.3794(2) 0.26536(19) 1.14218(17) 0.0203(4) Uani 1 1 d .
O8 O 0.3721(3) 0.4812(2) 1.28578(18) 0.0248(4) Uani 1 1 d .
O2 O 0.3197(3) 0.9253(2) 1.0751(2) 0.0351(5) Uani 1 1 d .
O3 O 0.0241(3) 0.8481(2) 0.9068(2) 0.0374(5) Uani 1 1 d .
O1 O 0.3071(3) 0.8820(2) 0.82191(19) 0.0266(4) Uani 1 1 d .
O5 O -0.0770(3) 0.2614(3) 0.5422(2) 0.0432(6) Uani 1 1 d .
O4 O 0.2407(3) 0.3715(2) 0.53063(19) 0.0306(4) Uani 1 1 d .
O6 O 0.1559(3) 0.1396(2) 0.6179(2) 0.0351(5) Uani 1 1 d .
O9 O 0.5665(2) 0.29661(19) 0.43102(17) 0.0202(4) Uani 1 1 d .
H9A H 0.6622 0.2868 0.4853 0.044 Uiso 1 1 d .
O10 O 0.4862(3) 1.0374(2) 0.62438(19) 0.0274(4) Uani 1 1 d .
H10A H 0.3891 1.0673 0.6236 0.060 Uiso 1 1 d .
O11 O 0.8261(3) 0.9385(2) 0.6972(2) 0.0320(4) Uani 1 1 d .
H11A H 0.9091 0.9242 0.7643 0.076 Uiso 1 1 d .
H11B H 0.8761 0.9858 0.6357 0.082 Uiso 1 1 d .
S1 S 0.21175(7) 0.84006(6) 0.93455(6) 0.01495(16) Uani 1 1 d .
S2 S 0.11444(8) 0.28127(6) 0.60431(6) 0.01640(16) Uani 1 1 d .
H10B H 0.5000 1.0000 0.5000 0.10(2) Uiso 1 2 d S
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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sc Sc 0.3119 1.5331 '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
O9 Sc2 O9 180.0 2_666 .
O9 Sc2 O8 91.70(6) 2_666 1_554
O9 Sc2 O8 88.30(6) . 1_554
O9 Sc2 O8 88.30(6) 2_666 2_667
O9 Sc2 O8 91.70(6) . 2_667
O8 Sc2 O8 180.0 1_554 2_667
O9 Sc2 O4 90.33(7) 2_666 2_666
O9 Sc2 O4 89.67(7) . 2_666
O8 Sc2 O4 90.92(7) 1_554 2_666
O8 Sc2 O4 89.08(7) 2_667 2_666
O9 Sc2 O4 89.67(7) 2_666 .
O9 Sc2 O4 90.33(7) . .
O8 Sc2 O4 89.08(7) 1_554 .
O8 Sc2 O4 90.92(7) 2_667 .
O4 Sc2 O4 180.00(10) 2_666 .
O10 Sc1 O9 92.67(7) . 2_666
O10 Sc1 O7 179.52(7) . 2_667
O9 Sc1 O7 87.14(7) 2_666 2_667
O10 Sc1 O1 88.92(7) . .
O9 Sc1 O1 97.05(7) 2_666 .
O7 Sc1 O1 91.54(7) 2_667 .
O10 Sc1 O11 91.29(8) . .
O9 Sc1 O11 95.85(7) 2_666 .
O7 Sc1 O11 88.29(7) 2_667 .
O1 Sc1 O11 167.08(8) . .
O10 Sc1 O2 90.99(8) . 2_677
O9 Sc1 O2 176.32(7) 2_666 2_677
O7 Sc1 O2 89.19(7) 2_667 2_677
O1 Sc1 O2 83.31(8) . 2_677
O11 Sc1 O2 83.76(8) . 2_677
O7 C1 O8 124.5(2) . .
O7 C1 C2 117.6(2) . .
O8 C1 C2 118.0(2) . .
C7 C2 C3 120.5(2) . .
C7 C2 C1 119.5(2) . .
C3 C2 C1 119.9(2) . .
C4 C3 C2 118.4(2) . .
C5 C4 C3 121.9(2) . .
C5 C4 S1 116.53(18) . .
C3 C4 S1 121.40(18) . .
C6 C5 C4 118.4(2) . .
C5 C6 C7 121.2(2) . .
C5 C6 S2 117.02(18) . .
C7 C6 S2 121.62(18) . .
C6 C7 C2 119.5(2) . .
C1 O7 Sc1 138.89(15) . 2_667
C1 O8 Sc2 138.82(16) . 1_556
S1 O2 Sc1 161.24(13) . 2_677
S1 O1 Sc1 144.82(12) . .
S2 O4 Sc2 156.29(13) . .
Sc1 O9 Sc2 133.49(8) 2_666 .
H10B O10 Sc1 111.31(11) . .
O3 S1 O2 114.05(13) . .
O3 S1 O1 111.30(12) . .
O2 S1 O1 111.75(12) . .
O3 S1 C4 108.58(11) . .
O2 S1 C4 105.64(11) . .
O1 S1 C4 104.89(10) . .
O5 S2 O6 114.06(14) . .
O5 S2 O4 111.27(13) . .
O6 S2 O4 112.30(12) . .
O5 S2 C6 107.49(11) . .
O6 S2 C6 106.91(11) . .
O4 S2 C6 104.09(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Sc2 O9 2.0853(16) 2_666
Sc2 O9 2.0853(16) .
Sc2 O8 2.1054(16) 1_554
Sc2 O8 2.1054(16) 2_667
Sc2 O4 2.1118(18) 2_666
Sc2 O4 2.1118(18) .
Sc1 O10 2.0127(17) .
Sc1 O9 2.0473(16) 2_666
Sc1 O7 2.1027(16) 2_667
Sc1 O1 2.1169(18) .
Sc1 O11 2.1317(18) .
Sc1 O2 2.1445(19) 2_677
C1 O7 1.259(3) .
C1 O8 1.263(3) .
C1 C2 1.495(3) .
C2 C7 1.393(3) .
C2 C3 1.394(3) .
C3 C4 1.392(4) .
C4 C5 1.388(3) .
C4 S1 1.762(2) .
C5 C6 1.385(3) .
C6 C7 1.386(4) .
C6 S2 1.773(2) .
O7 Sc1 2.1027(16) 2_667
O8 Sc2 2.1054(16) 1_556
O2 S1 1.4413(19) .
O2 Sc1 2.1445(19) 2_677
O3 S1 1.4255(19) .
O1 S1 1.4569(18) .
O5 S2 1.429(2) .
O4 S2 1.4619(18) .
O6 S2 1.4414(19) .
O9 Sc1 2.0473(16) 2_666
O10 H10B 1.2223(17) .
