Synthesis and Characterization of a New Three-Dimensional Lanthanide Carboxyphosphonate: Ln4(H2O)7[O2C-C5H10N-CH2-PO3]4(H2O)5
Christian Serre; Norbert Stock; Thomas Bein; Gérard Férey; Inorganic Chemistry 43 (2004) 3159–3163; doi:10.1021/ic035363p

data_4310999
_publ_contact_author             'SERRE Christian'
_publ_contact_author_email       serre@chimie.uvsq.fr
_publ_section_title
;
 Synthesis and Characterization of a New Three-Dimensional Lanthanide
 Carboxyphosphonate: Ln4(H2O)7[O2C-C5H10N-CH2-PO3]4(H2O)5
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3159
_journal_page_last               3163
_journal_paper_doi               10.1021/ic035363p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C112 H80 N16 O128 P16 Pr16'
_chemical_formula_weight         6448
_chemical_name_common            MIL84
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2003-11-14T12:49:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 105.63
_cell_angle_gamma                90
_cell_formula_units_Z            1
_cell_length_a                   23.4805(10)
_cell_length_b                   10.1588(10)
_cell_length_c                   23.0055(10)
_cell_measurement_temperature    293(2)
_cell_volume                     5284.7(6)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Shelxs 97'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.472
_diffrn_measured_fraction_theta_max 0.472
_diffrn_measurement_device
'Enraf-Nonius Kappa CCD equipped with a rotating anode'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0674
_diffrn_reflns_av_unetI/netI     0.0854
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            16414
_diffrn_reflns_theta_full        27.39
_diffrn_reflns_theta_max         27.39
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'Mo source'
_exptl_absorpt_coefficient_mu    3.837
_exptl_crystal_colour            'light green'
_exptl_crystal_density_diffrn    'not measured'
_exptl_crystal_density_meas      2.05
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'rod-like shape'
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.025
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.701
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.42(2)
_refine_ls_extinction_coef       0.00035(4)
_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   1.127
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     314
_refine_ls_number_reflns         5497
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0681
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+38.3989P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0983
_reflns_number_gt                4599
_reflns_number_total             5497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035363psi20031125_045407.cif
_cod_data_source_block           compound(1)-Cc
_cod_original_cell_volume        5284.6(6)
_cod_database_code               4310999