The Structure of a Complex Open-Framework Germanate Obtained by Combining Powder Charge-Flipping and Simulated Annealing
Inge, A. Ken; Huang, Shiliang; Chen, Hong; Moraga, Francisca; Sun, Junliang; Zou, Xiaodong; Crystal Growth & Design 12 (2012) 4853–; doi:10.1021/cg300647s

data_4506688
_publ_section_title
;
 The Structure of a Complex Open-Framework Germanate Obtained by
 Combining Powder Charge-Flipping and Simulated Annealing
;
_journal_issue                   10
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              4853
_journal_paper_doi               10.1021/cg300647s
_journal_volume                  12
_journal_year                    2012
_chemical_formula_moiety         Ge12H2O27,C6H17N3,2(H4N)
_chemical_formula_sum            'C6 H27 Ge12 N5 O27'
_chemical_formula_weight         1472.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 115.870(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.6277(10)
_cell_length_b                   17.3845(11)
_cell_length_c                   16.305(2)
_cell_measurement_reflns_used    10202
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.2557
_cell_measurement_theta_min      1.6698
_cell_volume                     3220.7(6)
_computing_cell_refinement
;
        CrysAlisPro, Oxford Diffraction Ltd.,
        Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET)
        (compiled Dec  8 2009,17:31:18)
;
_computing_data_collection
;                                                    
        CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009) 
;
_computing_data_reduction
;
         CrysAlisPro, Oxford Diffraction Ltd., 
         Version 1.171.34.9 (release 08-12-2009 CrysAlis171 .NET) 
         (compiled Dec  8 2009,17:31:18) 
;
_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 0.966
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Diamond Light Source Beamline I19'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.1873
_diffrn_reflns_av_sigmaI/netI    0.1869
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            21060
_diffrn_reflns_theta_full        24.21
_diffrn_reflns_theta_max         24.21
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    9.994
_exptl_absorpt_correction_T_max  0.9425
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_process_details
;                                                          
CrysAlis RED, Oxford Diffraction Ltd.,                     
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET)  
(compiled Jan 10 2008,16:37:18)                            
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm.          
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    3.037
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blcok
_exptl_crystal_F_000             2792
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.012
_refine_diff_density_max         3.205
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.363
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.998
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     438
_refine_ls_number_reflns         5497
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0780
_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^)+(0.0719P)^2^+7.8956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2010
_refine_ls_wR_factor_ref         0.2201
_reflns_number_gt                4204
_reflns_number_total             5497
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg300647s_si_002.cif
_cod_data_source_block           1760
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        3220.7(5)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4506688