Investigation of the GeO2-1,6-Diaminohexane-Water-Pyridine-HF Phase Diagram Leading to the Discovery of Two Novel Layered Germanates with Extra-Large Rings
Bing Guo; Andrew K. Inge; Charlotte Bonneau; Junliang Sun; Kirsten E. Christensen; Zhong-Yong Yuan; Xiaodong Zou; Inorganic Chemistry 50 (2011) 201–207; doi:10.1021/ic1017505

data_4324111
_publ_section_title
;
 Investigation of the GeO2-1,6-Diaminohexane-Water-Pyridine-HF Phase
 Diagram Leading to the Discovery of Two Novel Layered Germanates with
 Extra-Large Rings
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              201
_journal_page_last               207
_journal_paper_doi               10.1021/ic1017505
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'Ge21 O51'
_chemical_formula_weight         2340.39
_chemical_name_common            SU-63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           185
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  'P 6c -2'
_symmetry_space_group_name_H-M   'P 63 c m'
_atom_sites_solution_hydrogens   none
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   28.794(2)
_cell_length_b                   28.794(2)
_cell_length_c                   20.603(4)
_cell_measurement_reflns_used    4988
_cell_measurement_temperature    106(2)
_cell_measurement_theta_max      27.23
_cell_measurement_theta_min      2.58
_cell_volume                     14793(3)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_molecular_graphics    CrystalMake
_computing_publication_material  CrystalMake
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      106(2)
_diffrn_detector_area_resol_mean 12.613
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device       'MARCCD, MARDTB Phi-Axis Goniometer'
_diffrn_measurement_device_type  MarDTB
_diffrn_measurement_method       'profile data'
_diffrn_measurement_specimen_support 'glass fiber'
_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  'graphite 002'
_diffrn_radiation_polarisn_norm  0.00
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.90800
_diffrn_reflns_av_R_equivalents  0.0954
_diffrn_reflns_av_sigmaI/netI    0.0790
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            51182
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_full        33.84
_diffrn_reflns_theta_max         33.84
_diffrn_reflns_theta_min         3.04
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.353
_exptl_absorpt_correction_T_max  0.8835
_exptl_absorpt_correction_T_min  0.4491
_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:  8  and  1
   Point group:  622
   Friedel opposites are not equivalent.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_platon_squeeze_details
;
;
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.024
_refine_diff_density_rms         0.192
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.0(3)
_refine_ls_extinction_coef       0.00314(19)
_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   1.030
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.1112
_refine_ls_R_factor_gt           0.0851
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1507P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2163
_refine_ls_wR_factor_ref         0.2422
_reflns_number_gt                5624
_reflns_number_total             8692
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1017505_si_002_1.cif
_cod_data_source_block           SU-63
_cod_database_code               4324111