A Flexible Germanate Structure Containing 24-Ring Channels and with Very Low Framework Density
Jacques Plévert; Travis M. Gentz; Aaron Laine; Hailian Li; Victor G. Young; Omar M. Yaghi; Michael O'Keeffe; Journal of the American Chemical Society 123 (2001) 12706–12707; doi:10.1021/ja016996a

data_4115855
_publ_section_title
;
 A Flexible Germanate Structure Containing 24-Ring Channels and with Very
 Low Framework Density
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12706
_journal_page_last               12707
_journal_paper_doi               10.1021/ja016996a
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C6 H18 F4 Ge14 N3 O32'
_chemical_formula_weight         2153.06
_chemical_name_common            ASU-16
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           23
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 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            8
_cell_length_a                   16.9109(8)
_cell_length_b                   24.267(2)
_cell_length_c                   30.210(3)
_cell_measurement_temperature    120(2)
_cell_volume                     12397.5(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Kappa CCD'
_diffrn_measurement_method       'Phi scans'
_diffrn_radiation_monochromator  'Silicon plus mirrors'
_diffrn_radiation_source         'APS 15-ID-C'
_diffrn_radiation_type           X-rays
_diffrn_radiation_wavelength     0.55940
_diffrn_reflns_av_R_equivalents  0.0634
_diffrn_reflns_av_sigmaI/netI    0.0695
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            50669
_diffrn_reflns_theta_full        19.49
_diffrn_reflns_theta_max         19.49
_diffrn_reflns_theta_min         0.85
_exptl_absorpt_coefficient_mu    3.571
_exptl_absorpt_correction_T_max  0.9652
_exptl_absorpt_correction_T_min  0.7166
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2.03, Sheldrick, (1999)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    2.307
_exptl_crystal_description       Needle
_exptl_crystal_F_000             8408
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.920
_refine_diff_density_min         -1.353
_refine_diff_density_rms         0.152
_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_method     none
_refine_ls_goodness_of_fit_ref   0.967
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         10948
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0385
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0924
_reflns_number_gt                8984
_reflns_number_total             10948
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja016996a_s1.cif
_cod_data_source_block           ASU-16
_cod_original_cell_volume        12397.6(16)
_cod_database_code               4115855