Soft-Hard Acid-Base Interactions: Probing Coordination Preferences of Sulfur and Selenium in Mixed Chalcophosphates in the Family APbPS4-xSex (A = K, Rb, Cs; x= 0-4)
Alexander Rothenberger; Collin Morris; Hsien-Hau Wang; Duck Young Chung; Mercouri G. Kanatzidis; Inorganic Chemistry 48 (2009) 9036–9040; doi:10.1021/ic901283k

data_4303208
_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
;
Soft-Hard Acid-Base Interactions: Probing Coordination Preferences of
Sulfur and Selenium in Mixed Chalcophosphates in the Family APbPS4-xSex (A
= K, Rb, Cs; x= 0-4)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9036
_journal_page_last               9040
_journal_paper_doi               10.1021/ic901283k
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'K P Pb S1.84 Se2.16'
_chemical_formula_weight         506.92
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   undef
_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                   17.0617(12)
_cell_length_b                   6.6134(6)
_cell_length_c                   6.7435(5)
_cell_measurement_reflns_used    7482
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.54
_cell_measurement_theta_min      3.35
_cell_volume                     760.91(10)
_computing_cell_refinement       'stoe x-area'
_computing_data_collection       'stoe x-area'
_computing_data_reduction        'stoe x-area'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'stoe ipds 2t'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0285
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6214
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.17
_diffrn_reflns_theta_min         3.85
_exptl_absorpt_coefficient_mu    33.664
_exptl_absorpt_correction_T_max  0.5525
_exptl_absorpt_correction_T_min  0.4316
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'stoe x-red32'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    4.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             876
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.285
_refine_diff_density_min         -2.829
_refine_diff_density_rms         0.307
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.493(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     55
_refine_ls_number_reflns         2011
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0285P)^2^+8.5784P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                1912
_reflns_number_total             2011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901283k_si_002_2.cif
_cod_data_source_block           1
_cod_database_code               4303208