Molecular Germanium Selenophosphate Salts: Phase-Change Properties and Strong Second Harmonic Generation
Collin D. Morris; In Chung; Sungoh Park; Connor M. Harrison; Daniel J. Clark; Joon I. Jang; Mercouri G. Kanatzidis; Journal of the American Chemical Society 134 (2012) 20733–20744; doi:10.1021/ja309386e

data_4119041
_publ_section_title
;
 Molecular Germanium Selenophosphate Salts: Phase-Change Properties and
 Strong Second Harmonic Generation
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20733
_journal_page_last               20744
_journal_paper_doi               10.1021/ja309386e
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'Ge P4 Se12, 4(K)'
_chemical_formula_sum            'Ge K4 P4 Se12'
_chemical_formula_weight         1300.39
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_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                   13.9465(4)
_cell_length_b                   7.2435(2)
_cell_length_c                   24.0511(9)
_cell_measurement_reflns_used    20532
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.22
_cell_measurement_theta_min      2.81
_cell_volume                     2429.68(13)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       w-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  0.0727
_diffrn_reflns_av_sigmaI/netI    0.0504
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            22093
_diffrn_reflns_theta_full        29.00
_diffrn_reflns_theta_max         29.00
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    20.174
_exptl_absorpt_correction_T_max  0.6007
_exptl_absorpt_correction_T_min  0.0257
_exptl_absorpt_correction_type   integration
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.555
_exptl_crystal_description       rod
_exptl_crystal_F_000             2304
_exptl_crystal_size_max          0.7153
_exptl_crystal_size_mid          0.0449
_exptl_crystal_size_min          0.0270
_refine_diff_density_max         0.874
_refine_diff_density_min         -1.525
_refine_diff_density_rms         0.218
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         5819
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0747P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                5303
_reflns_number_total             5819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja309386e_si_002_4.cif
_cod_data_source_block           k4gep4se12
_cod_original_cell_volume        2429.68(17)
_cod_database_code               4119041