An Open-Framework Silicogermanate with 26-Ring Channels Built from Seven-Coordinated (Ge,Si)10(O,OH)28 Clusters
Kirsten E. Christensen; Charlotte Bonneau; Mikaela Gustafsson; Lei Shi; Junliang Sun; Jekabs Grins; Kjell Jansson; Isabelle Sbille; Bao-Lian Su; Xiadong Zou; Journal of the American Chemical Society 130 (2008) 3758–3759; doi:10.1021/ja8002556

data_4107604
_publ_section_title
;
 An Open-Framework Silicogermanate with 26-Ring Channels Built from
 Seven-Coordinated (Ge,Si)10(O,OH)28 Clusters
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3758
_journal_page_last               3759
_journal_paper_doi               10.1021/ja8002556
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'Ge39.56 O118 Si12.44, 16(N)'
_chemical_formula_sum            'Ge39.56 N16 O118 Si12.44'
_chemical_formula_weight         5330.59
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2008-01-09T14:10:57-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   34.476(3)
_cell_length_b                   19.8768(17)
_cell_length_c                   14.8594(8)
_cell_measurement_reflns_used    5809
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.94
_cell_measurement_theta_min      1.48
_cell_measurement_wavelength     0.907
_cell_volume                     10182.7(14)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 '  CCD'
_diffrn_detector_area_resol_mean 13.653
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device       'MARCCD, MARDTB Phi-Axis Goniometer'
_diffrn_measurement_device_type  '  MarDTB'
_diffrn_measurement_method       'profile data'
_diffrn_orient_matrix_type
;  x  =  h UB
   coordinate system:
     x from crystal towards source
     z vertical, towards goniometer base
     y so that x,y,z is right-handed
;
_diffrn_orient_matrix_UB_11      -0.057962
_diffrn_orient_matrix_UB_12      0.00097
_diffrn_orient_matrix_UB_13      0.001892
_diffrn_orient_matrix_UB_21      -0.028927
_diffrn_orient_matrix_UB_22      -0.043261
_diffrn_orient_matrix_UB_23      0.025793
_diffrn_orient_matrix_UB_31      0.00246
_diffrn_orient_matrix_UB_32      0.033189
_diffrn_orient_matrix_UB_33      0.058493
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.907
_diffrn_reflns_av_R_equivalents  0.1543
_diffrn_reflns_av_unetI/netI     0.0519
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            59924
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        33.12
_diffrn_reflns_theta_max         33.12
_diffrn_reflns_theta_min         6.82
_exptl_absorpt_coefficient_mu    11.054
_exptl_absorpt_correction_T_max  0.9782
_exptl_absorpt_correction_T_min  0.4044
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;  Shape and scale corrections using equivalent reflections.
   Shape function based on spherical harmonics.
   Highest even and odd order for spherical harmonics:  4  and  1
   Laue group:  -1
   Friedel opposites are equivalent.
;
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_F_000             4990
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.015
_exptl_crystal_size_min          0.002
_refine_diff_density_max         2.256
_refine_diff_density_min         -1.367
_refine_diff_density_rms         0.212
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4827
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0563
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+27.9277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1496
_refine_ls_wR_factor_ref         0.159
_reflns_number_gt                3881
_reflns_number_total             4827
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja8002556-file003.cif
_cod_data_source_block           new
_cod_database_code               4107604