Synthesis, Single-Crystal X-ray Microdiffraction, and NMR Characterizations of the Giant Pore Metal-Organic Framework Aluminum Trimesate MIL-100
Volkringer, Christophe; Popov, Dimitry; Loiseau, Thierry; Férey, Gérard; Burghammer, Manfred; Riekel, Christian; Haouas, Mohamed; Taulelle, Francis; Chemistry of Materials 21 (2009) 5695–; doi:10.1021/cm901983a

data_4001058
_publ_section_title
;
 Synthesis, Single-Crystal X-ray Microdiffraction, and NMR
 Characterizations of the Giant Pore Metal-Organic Framework Aluminum
 Trimesate MIL-100
;
_journal_issue                   24
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5695
_journal_paper_doi               10.1021/cm901983a
_journal_volume                  21
_journal_year                    2009
_chemical_formula_sum            'C306 H102 Al51 O374'
_chemical_formula_weight         11137.86
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           227
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  '-F 4vw 2vw 3'
_symmetry_space_group_name_H-M   'F d -3 m :2'
_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            16
_cell_length_a                   71.687(3)
_cell_length_b                   71.687(3)
_cell_length_c                   71.687(3)
_cell_measurement_reflns_used    5484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.7
_cell_measurement_theta_min      1.7
_cell_volume                     368401(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.899
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'ESRF ID13 goniometer setup'
_diffrn_measurement_method       'oscillating method'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.96120
_diffrn_reflns_av_R_equivalents  0.3635
_diffrn_reflns_av_sigmaI/netI    0.1432
_diffrn_reflns_limit_h_max       71
_diffrn_reflns_limit_h_min       -66
_diffrn_reflns_limit_k_max       71
_diffrn_reflns_limit_k_min       -63
_diffrn_reflns_limit_l_max       71
_diffrn_reflns_limit_l_min       -66
_diffrn_reflns_number            110248
_diffrn_reflns_theta_full        28.72
_diffrn_reflns_theta_max         28.72
_diffrn_reflns_theta_min         1.67
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.105
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    0.803
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             76432
_exptl_crystal_size_max          0.002
_exptl_crystal_size_mid          0.002
_exptl_crystal_size_min          0.002
_refine_diff_density_max         1.015
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.441
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         7888
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.441
_refine_ls_R_factor_all          0.2279
_refine_ls_R_factor_gt           0.1744
_refine_ls_shift/su_max          3.546
_refine_ls_shift/su_mean         0.206
_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          0.4014
_refine_ls_wR_factor_ref         0.4298
_reflns_number_gt                5267
_reflns_number_total             7888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm901983a_si_001.cif
_cod_data_source_block           shelxl
_cod_original_cell_volume        368401(27)
_cod_original_sg_symbol_H-M      f_d_-3_m
_cod_database_code               4001058