MIL-50, an Open-Framework GaPO with a Periodic Pattern of Small Water Ponds and Dry Rubidium Atoms: a Combined XRD, NMR, and Computational Study
Lionel Beitone; Jérôme Marrot; Thierry Loiseau; Gérard Férey; Marc Henry; Clarisse Huguenard; Axel Gansmuller; Francis Taulelle; Journal of the American Chemical Society 125 (2003) 1912–1922; doi:10.1021/ja029072b

data_4113465
_publ_section_title
;
 MIL-50, an Open-Framework GaPO with a Periodic Pattern of Small Water
 Ponds and Dry Rubidium Atoms: a Combined XRD, NMR, and Computational
 Study
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1912
_journal_page_last               1922
_journal_paper_doi               10.1021/ja029072b
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C12 H37 F7 Ga9 N4 O40.5 P9 Rb2'
_chemical_formula_weight         2095.61
_chemical_name_common            MIL-50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           36
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c -2'
_symmetry_space_group_name_H-M   'C m c 21'
_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                   32.1510(2)
_cell_length_b                   17.2290(3)
_cell_length_c                   10.2120(1)
_cell_measurement_reflns_used    8851
_cell_measurement_temperature    296(2)
_cell_volume                     5656.73(12)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0635
_diffrn_reflns_av_sigmaI/netI    0.0736
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12997
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.27
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.308
_exptl_absorpt_correction_T_max  0.9396
_exptl_absorpt_correction_T_min  0.1446
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.461
_exptl_crystal_description       needle
_exptl_crystal_F_000             4048
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.821
_refine_diff_density_min         -1.215
_refine_diff_density_rms         0.438
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.03(2)
_refine_ls_extinction_coef       0.00139(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   1.161
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4144
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0509
_refine_ls_shift/su_max          0.075
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0778P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1423
_reflns_number_gt                3504
_reflns_number_total             4144
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja029072b_s1.cif
_cod_data_source_block           52sa
_cod_original_cell_volume        5656.69(10)
_cod_original_formula_sum        'C12 H37 F7 Ga9 N4 O40.50 P9 Rb2'
_cod_database_code               4113465