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_4324112
_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            'C42 Ge51 N14 O136'
_chemical_formula_weight         6578.65
_chemical_name_common            SU-64
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.861(11)
_cell_angle_beta                 89.500(17)
_cell_angle_gamma                83.173(13)
_cell_formula_units_Z            1
_cell_length_a                   12.101(4)
_cell_length_b                   18.113(6)
_cell_length_c                   22.444(8)
_cell_measurement_reflns_used    15340
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.5
_cell_measurement_theta_min      1.4
_cell_volume                     4881(3)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.762
_diffrn_measured_fraction_theta_max 0.762
_diffrn_measurement_device
;
CrystalLogic Kappa (3 circle)
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \f-scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1435
_diffrn_reflns_av_sigmaI/netI    0.1762
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42228
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.38
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.817
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.566
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3070
_exptl_crystal_size_max          0.030
_exptl_crystal_size_mid          0.008
_exptl_crystal_size_min          0.002
_platon_squeeze_details
;
;
_refine_diff_density_max         2.042
_refine_diff_density_min         -2.321
_refine_diff_density_rms         0.409
_refine_ls_extinction_coef       0.00025(7)
_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   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     617
_refine_ls_number_reflns         15210
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1922
_refine_ls_R_factor_gt           0.1296
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1590P)^2^+297.9275P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3363
_refine_ls_wR_factor_ref         0.3799
_reflns_number_gt                8159
_reflns_number_total             15210
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1017505_si_002_2.cif
_cod_data_source_block           su64p2
_cod_database_code               4324112