Germanium Selenophosphates: The Incommensurately Modulated 1/\ιnfty[Ge4-xPxSe124-] and the Molecular [Ge2P2Se14]6-
Collin D. Morris; Christos D. Malliakas; Mercouri G. Kanatzidis; Inorganic Chemistry 50 (2011) 10241–10248; doi:10.1021/ic201249w

data_4326519
_publ_contact_author
;
      Prof. M. G. Kanatzidis
      Department of Chemistry
      2145 Sheridan Road
      Northwestern University
      Evanston, IL 60208-3113
      USA
;
_publ_contact_author_email       m-kanatzidis@northwestern.edu
_publ_contact_author_fax         'Int + 847-491-5937'
_publ_contact_author_phone       'Int + 847-467-1541'
_publ_section_title
;
 Germanium Selenophosphates: The Incommensurately Modulated
 1/\\infty[Ge4-xPxSe124-] and the Molecular [Ge2P2Se14]6-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10241
_journal_page_last               10248
_journal_paper_doi               10.1021/ic201249w
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'Ge2.54 P1.46 Se8, 4(Se), 4(K)'
_chemical_formula_sum            'Ge2.54 K4 P1.46 Se12'
_chemical_formula_weight         1311.04
_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_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.025(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            1
_cell_length_a                   6.7388(7)
_cell_length_b                   13.4894(12)
_cell_length_c                   6.3904(6)
_cell_measurement_reflns_used    9993
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.62
_cell_measurement_theta_min      3.02
_cell_volume                     580.81(10)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       rotation
_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  0.0455
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5044
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    22.228
_exptl_absorpt_correction_T_max  0.4360
_exptl_absorpt_correction_T_min  0.0866
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    3.748
_exptl_crystal_description       rod
_exptl_crystal_F_000             578
_exptl_crystal_size_max          0.2414
_exptl_crystal_size_mid          0.0925
_exptl_crystal_size_min          0.0749
_refine_diff_density_max         0.827
_refine_diff_density_min         -1.407
_refine_diff_density_rms         0.199
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.240
_refine_ls_matrix_type           full
_refine_ls_number_parameters     57
_refine_ls_number_reflns         1555
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.240
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0176P)^2^+3.9986P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0760
_reflns_number_gt                1443
_reflns_number_total             1555
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201249w_si_002_1.cif
_cod_data_source_block           K4Ge2.54P1.46Se12
_cod_database_code               4326519