Dryness sensitive porous 3d‒4f metal‒organic framework with unusual dynamic behaviour
Fabelo, Oscar; Cañadillas-Delgado, Laura; Pasán, Jorge; Díaz-Gallifa, Pau; Labrador, Ana; Ruiz-Pérez, Catalina; CrystEngComm 14 (2012) 765–; doi:10.1039/c1ce06210g

data_7207202
_publ_section_title
;
 Dryness sensitive porous 3d--4f metal--organic framework with unusual
 dynamic behaviour
;
_journal_issue                   3
_journal_name_full               CrystEngComm
_journal_page_first              765
_journal_paper_doi               10.1039/c1ce06210g
_journal_volume                  14
_journal_year                    2012
_chemical_formula_sum            'C25 H45 Cu2 O40 Pr2'
_chemical_formula_weight         1394.51
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 99.88(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.953(2)
_cell_length_b                   23.056(5)
_cell_length_c                   19.811(4)
_cell_measurement_temperature    293(2)
_cell_volume                     4928.7(18)
_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      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7383
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            90569
_diffrn_reflns_theta_full        28.92
_diffrn_reflns_theta_max         28.92
_diffrn_reflns_theta_min         1.37
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    3.194
_exptl_absorpt_correction_T_max  0.8684
_exptl_absorpt_correction_T_min  0.7600
_exptl_absorpt_correction_type   sphere
_exptl_crystal_colour            light_blue
_exptl_crystal_density_diffrn    1.879
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2764
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.972
_refine_diff_density_min         -1.472
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       0.00051(12)
_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   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         11573
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0494
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+23.0827P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1633
_reflns_number_gt                9974
_reflns_number_total             11573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1ce06210g.txt
_cod_data_source_block           1a
_cod_original_cell_volume        4929.0(17)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7207202