Open-Framework Germanate Built from the Hexagonal Packing of Rigid Cylinders
Charlotte Bonneau; Junliang Sun; Rebeca Sanchez-Smith; Bing Guo; Daliang Zhang; Andrew Kentaro Inge; Mattias Edén; Xiaodong Zou; Inorganic Chemistry 48 (2009) 9962–9964; doi:10.1021/ic900940s

data_4303442
_publ_section_title
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Open-Framework Germanate Built from the Hexagonal Packing of Rigid Cylinders
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9962
_journal_page_last               9964
_journal_paper_doi               10.1021/ic900940s
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C18 H46 Ge33 N8 O75'
_chemical_formula_weight         3970.10
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_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                   49.257(10)
_cell_length_b                   28.439(6)
_cell_length_c                   14.866(3)
_cell_measurement_reflns_used    8092
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.49
_cell_measurement_theta_min      1.21
_cell_volume                     20825(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 12.652
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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_radiation_monochromator  'Bent silicon crystal, horizontally focusing'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Multi-pole wiggler'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.03
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.1230
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            30028
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        30.99
_diffrn_reflns_theta_max         30.99
_diffrn_reflns_theta_min         5.50
_exptl_absorpt_coefficient_mu    24.782
_exptl_absorpt_correction_T_max  0.8655
_exptl_absorpt_correction_T_min  0.3704
_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
 Symmetry information for component no. 1:
   Laue group:  6/mmm
   Friedel opposites are equivalent.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.540
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             14928
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.006
_platon_squeeze_details
;
;
_refine_diff_density_max         2.578
_refine_diff_density_min         -2.955
_refine_diff_density_rms         0.366
_refine_ls_extinction_coef       0.000049(8)
_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   0.943
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     372
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      0.943
_refine_ls_R_factor_all          0.1217
_refine_ls_R_factor_gt           0.0749
_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^)+(0.1136P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1892
_refine_ls_wR_factor_ref         0.2054
_reflns_number_gt                3120
_reflns_number_total             5933
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic900940s_si_002.cif
_cod_data_source_block           ASU-21
_cod_database_code               4303442