Ammonothermal Crystal Growth of Germanium and Its Alloys: Synthesis of a Hollow Metallic Crystal
Purdy, Andrew P.; Case, Sean; George, Clifford; Crystal Growth & Design 3 (2003) 121–; doi:10.1021/cg025590m

data_4505654
_publ_section_title
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 Ammonothermal Crystal Growth of Germanium and Its Alloys:&#x2009;
 Synthesis of a Hollow Metallic Crystal
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              121
_journal_paper_doi               10.1021/cg025590m
_journal_volume                  3
_journal_year                    2003
_chemical_formula_sum            'Ge H3 N O8 Sn6'
_chemical_formula_weight         929.76
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           196
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'F 2 2 3'
_symmetry_space_group_name_H-M   'F 2 3'
_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            4
_cell_length_a                   10.4959(6)
_cell_length_b                   10.4959(6)
_cell_length_c                   10.4959(6)
_cell_measurement_reflns_used    3980
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      34.16
_cell_measurement_theta_min      3.03
_cell_volume                     1156.27(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      93(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0875
_diffrn_reflns_av_sigmaI/netI    0.0386
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4511
_diffrn_reflns_theta_full        34.51
_diffrn_reflns_theta_max         34.51
_diffrn_reflns_theta_min         3.36
_diffrn_standards_decay_%        none
_exptl_absorpt_coefficient_mu    15.333
_exptl_absorpt_correction_T_max  0.631
_exptl_absorpt_correction_T_min  0.464
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    5.341
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1624
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.022
_refine_diff_density_min         -2.752
_refine_diff_density_rms         0.409
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.11(13)
_refine_ls_extinction_coef       0.00068(14)
_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   1.148
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     15
_refine_ls_number_reflns         413
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.148
_refine_ls_R_factor_all          0.0550
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0594P)^2^+93.6913P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1291
_refine_ls_wR_factor_ref         0.1299
_reflns_number_gt                403
_reflns_number_total             413
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg025590msi20021207_112638.cif
_cod_data_source_block           purscbb(3)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according
to /home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary
named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1156.3(1)
_cod_original_sg_symbol_H-M      F23
_cod_original_formula_sum        'H3 Ge N O8 Sn6'
_cod_database_code               4505654