H3O2 Bridging Ligand in a Metal-Organic Framework. Insight into the Aqua-Hydroxo\λeftarrow\ρightarrowHydroxyl Equilibrium: A Combined Experimental and Theoretical Study
Richard F. D'Vries; Victor A. de la Peña-O'Shea; Natalia Snejko; Marta Iglesias; Enrique Gutiérrez-Puebla; M. Angeles Monge; Journal of the American Chemical Society 135 (2013) 5782–5792; doi:10.1021/ja4005046

data_4119583
_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\\leftarrow\\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 H16 O23.13 S4 Sc3'
_chemical_formula_sum            'C14 H16 O23.13 S4 Sc3'
_chemical_formula_weight         817.48
_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                69.198(2)
_cell_angle_beta                 85.365(3)
_cell_angle_gamma                82.458(3)
_cell_formula_units_Z            1
_cell_length_a                   7.5148(12)
_cell_length_b                   9.5270(15)
_cell_length_c                   10.2296(16)
_cell_measurement_reflns_used    3017
_cell_measurement_temperature    571(2)
_cell_measurement_theta_max      28.86
_cell_measurement_theta_min      2.30
_cell_volume                     678.25(19)
_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      571(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5083
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    1.140
_exptl_absorpt_correction_T_max  0.8050
_exptl_absorpt_correction_T_min  0.7519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.001
_exptl_crystal_description       prism
_exptl_crystal_F_000             411
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.080
_refine_ls_extinction_coef       0.044(3)
_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   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         2338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0359P)^2^+0.8563P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0878
_reflns_number_gt                2015
_reflns_number_total             2338
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja4005046_si_003.cif
_cod_data_source_block           data2t
_cod_database_code               4119583