Convenient Synthesis of Aluminum and Gallium Phosphonate Cages
Christian R. Samanamu; Marilyn M. Olmstead; Jean-Luc Montchamp; Anne F. Richards; Inorganic Chemistry 47 (2008) 3879–3887; doi:10.1021/ic800023d

data_4304922
_publ_section_title
;
Convenient Synthesis of Aluminum and Gallium Phosphonate Cages
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3879
_journal_page_last               3887
_journal_paper_doi               10.1021/ic800023d
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H42 Al4 N4 O24 P4, 8(N O3), 7(H2 O)'
_chemical_formula_sum            'C20 H58 Al4 N12 O55 P4'
_chemical_formula_weight         1578.58
_chemical_name_common            '[(2PypoH)4Al4(OH2)12](NO3)8.7H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 114.604(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.7007(19)
_cell_length_b                   24.348(4)
_cell_length_c                   25.701(3)
_cell_measurement_temperature    213(2)
_cell_volume                     6088.2(17)
_computing_cell_refinement       'SAINT 5.65 (Bruker, 2003)'
_computing_data_collection       'SMART 5.054 (Bruker, 2003)'
_computing_data_reduction        'SAINT 5.65 (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_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  0.0893
_diffrn_reflns_av_sigmaI/netI    0.0957
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            30699
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.318
_exptl_absorpt_correction_T_max  0.996
_exptl_absorpt_correction_T_min  0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.10 (Sheldrick, 2003)'
_exptl_crystal_density_diffrn    1.722
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3256
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.669
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         11001
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0813P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1376
_refine_ls_wR_factor_ref         0.1667
_reflns_number_gt                6646
_reflns_number_total             11001
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800023d-file004.cif
_cod_data_source_block           cmpd3
_cod_original_cell_volume        6088.2(16)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4304922