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_4304923
_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
'          C38 H50 Cl12 Ga8 N6 O24, 2(Ga Cl4), 8(C4 H8 O)'
_chemical_formula_sum            'C70 H114 Cl20 Ga10 N6 O32 P6'
_chemical_formula_weight         3143.69
_chemical_name_common
' [(2pypo)4(2pypoH)2Ga8Cl12(H20)4(thf)2][GaCl4]2.8(thf) '
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                68.691(3)
_cell_angle_beta                 88.293(3)
_cell_angle_gamma                61.349(2)
_cell_formula_units_Z            1
_cell_length_a                   14.533(2)
_cell_length_b                   15.101(3)
_cell_length_c                   19.687(3)
_cell_measurement_reflns_used    5833
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      24.9
_cell_measurement_theta_min      2.20
_cell_volume                     3476.8(10)
_computing_cell_refinement       'Bruker SAINT+ v. 6.36a'
_computing_data_collection       'Bruker SMART v. 5.626'
_computing_data_reduction        'Bruker SAINT+ v. 6.36a'
_computing_molecular_graphics    'XP, Bruker SHELXTL v. 6.12'
_computing_publication_material  'XCIF, Bruker SHELXTL v. 6.12'
_computing_structure_refinement  'XL, Bruker SHELXTL v. 6.12'
_computing_structure_solution    'XS, Bruker SHELXTL v. 6.12'
_diffrn_ambient_temperature      213(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0597
_diffrn_reflns_av_sigmaI/netI    0.0920
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            29356
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    2.418
_exptl_absorpt_correction_T_max  0.972
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.501
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1572
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.650
_refine_diff_density_min         -1.373
_refine_diff_density_rms         0.178
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     588
_refine_ls_number_reflns         13492
_refine_ls_number_restraints     213
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.1578
_refine_ls_R_factor_gt           0.0793
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1361P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2385
_refine_ls_wR_factor_ref         0.2675
_reflns_number_gt                6956
_reflns_number_total             12481
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic800023d-file005.cif
_cod_data_source_block           ar387
_cod_database_code               4304923