Single-crystal XRD and solid-state NMR structural resolution of a layered fluorinated gallium phosphate: RbGa3(PO4)(2)(HPO4)F4·C5N2H16·2H2O (MIL-145).
Martineau, Charlotte; Loiseau, Thierry; Beitone, Lionel; Férey, Gérard; Bouchevreau, Boris; Taulelle, Francis; Dalton transactions (Cambridge, England : 2003) 42 (2013) 422–431; doi:10.1039/c2dt31464a

data_7020649
_publ_section_title
;
 Single-crystal XRD and solid-state NMR structural resolution of a layered
 fluorinated gallium phosphate:
 RbGa3(PO4)(2)(HPO4)F4&#x00B7;C5N2H16&#x00B7;2H2O (MIL-145).
;
_journal_issue                   2
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              422
_journal_page_last               431
_journal_paper_doi               10.1039/c2dt31464a
_journal_volume                  42
_journal_year                    2013
_chemical_absolute_configuration 'Flack H D (1983), Acta Cryst. A39, 876-881'
_chemical_formula_sum            'C20 H84 F16 Ga12 N8 O56 P12 Rb4'
_chemical_formula_weight         3187.11
_chemical_name_systematic
;
?
;
_space_group_IT_number           3
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2y'
_symmetry_space_group_name_H-M   'P 1 2 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                 112.7080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   14.4314(2)
_cell_length_b                   9.1152(2)
_cell_length_c                   16.78890(10)
_cell_measurement_reflns_used    5396
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      1.92
_cell_volume                     2037.30(6)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART/SAINT'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'Diamond 2.1e'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.913
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0464
_diffrn_reflns_av_sigmaI/netI    0.1090
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14513
_diffrn_reflns_theta_full        29.85
_diffrn_reflns_theta_max         29.85
_diffrn_reflns_theta_min         1.31
_exptl_absorpt_coefficient_mu    6.656
_exptl_absorpt_correction_T_max  0.7766
_exptl_absorpt_correction_T_min  0.6180
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'empirical (SADABS)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.598
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.01
_refine_diff_density_max         4.245
_refine_diff_density_min         -1.866
_refine_diff_density_rms         0.289
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.009(14)
_refine_ls_extinction_coef       0.00064(18)
_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   0.934
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9705
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.934
_refine_ls_R_factor_all          0.1107
_refine_ls_R_factor_gt           0.0611
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0723P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1583
_reflns_number_gt                5721
_reflns_number_total             9705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31464a.txt
_cod_data_source_block           lb1243_p2
_cod_original_cell_volume        2037.30(5)
_cod_original_sg_symbol_H-M      P2
_cod_database_code               7020649