Selective Gas and Vapor Sorption and Magnetic Sensing by an Isoreticular Mixed-Metal-Organic Framework
Jesús Ferrando-Soria; Pablo Serra-Crespo; Martijn de Lange; Jorge Gascon; Freek Kapteijn; Miguel Julve; Joan Cano; Francesc Lloret; Jorge Pasán; Catalina Ruiz-Pérez; Yves Journaux; Emilio Pardo; Journal of the American Chemical Society 134 (2012) 15301–15304; doi:10.1021/ja3045822

data_4118623
_publ_contact_author_address
;Laboratorio de Rayos X y Materiales Moleculares
 Dpto. F\'isica Fundamental II. Facultad de F\'isica
 Universidad de La Laguna
 E-38204. La Laguna. Tenerife
 Spain
;
_publ_contact_author_email       caruiz@ull.es
_publ_contact_author_fax         +34922318320
_publ_contact_author_name        'Professor Catalina Ruiz-P\'erez'
_publ_contact_author_phone       +34922318300
_publ_section_title
;
 Selective Gas and Vapor Sorption and Magnetic Sensing by an Isoreticular
 Mixed-Metal-Organic Framework
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15301
_journal_page_last               15304
_journal_paper_doi               10.1021/ja3045822
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Mn4, Cu6, Na4, 6(C13 H10 N2 O6), 60(H2 O)'
_chemical_formula_sum            'C78 H180 Cu6 Mn4 N12 Na4 O96'
_chemical_formula_weight         3514.34
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           123
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-P 4 2'
_symmetry_space_group_name_H-M   'P 4/m m m'
_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                   36.332(5)
_cell_length_b                   36.332(5)
_cell_length_c                   15.208(3)
_cell_measurement_temperature    100(2)
_cell_volume                     20075(6)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_wavelength     0.73850
_diffrn_reflns_av_R_equivalents  0.0960
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            306795
_diffrn_reflns_theta_full        25.75
_diffrn_reflns_theta_max         25.75
_diffrn_reflns_theta_min         1.30
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.3296
_exptl_absorpt_correction_T_min  0.3176
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       prism
_exptl_crystal_F_000             6792
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.543
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.273
_refine_ls_extinction_coef       0.017(2)
_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   2.870
_refine_ls_hydrogen_treatment    cosntr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     551
_refine_ls_number_reflns         9434
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      2.871
_refine_ls_R_factor_all          0.1911
_refine_ls_R_factor_gt           0.1906
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.5535
_refine_ls_wR_factor_ref         0.5536
_reflns_number_gt                9389
_reflns_number_total             9434
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3045822_si_001.cif
_cod_data_source_block           compound1
_cod_database_code               4118623
_exptl_absorpt_correction_t_ave  0.3245