Presence or Absence of a Central Se Atom in Silver Selenide/Selenolate Clusters with Halite Topology: Syntheses and Properties of [(Ph3PAg)8Ag6(μ6-Se)1-x/2(SePh)12]x+ (x= 0, 1)
Hari Pada Nayek; Werner Massa; Stefanie Dehnen; Inorganic Chemistry 49 (2010) 144–149; doi:10.1021/ic901629k

data_4314443
_publ_contact_author
;
Dehnen, S.

Fachbereich Chemie der Philipps-Universitaet
Hans-Meerwein-Str.
D-35043 Marburg, Germany
;
_publ_contact_author_email       dehnen@chemie.uni-marburg.de
_publ_contact_author_fax         +6421-2825653
_publ_contact_author_phone       +6421-2825751
_publ_section_title
;
 Presence or Absence of a Central Se Atom in Silver Selenide/Selenolate
 Clusters with Halite Topology: Syntheses and Properties of
 [(Ph3PAg)8Ag6(\m6-Se)1-x/2(SePh)12]x+ (x= 0, 1)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              144
_journal_page_last               149
_journal_paper_doi               10.1021/ic901629k
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety
'C216 H180 Ag14 P8 Se12.5, C18 H33 Cl2 Sn, 5(C4 H8 O)'
_chemical_formula_sum            'C254 H253 Ag14 Cl2 O5 P8 Se12.5 Sn'
_chemical_formula_weight         6320.09
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   20.3517(4)
_cell_length_b                   20.3517(4)
_cell_length_c                   99.087(3)
_cell_measurement_reflns_used    27007
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      1.225
_cell_volume                     35542.6(15)
_computing_cell_refinement       'XAREA 1.43 (Stoe 2007)'
_computing_data_collection       'XAREA 1.43 (Stoe 2007)'
_computing_data_reduction        'XAREA 1.43 (Stoe 2007)'
_computing_molecular_graphics    'DIAMOND 3.1f (Brandenburg 2007)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR 2004 (Burla et al. 2004)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 6.7
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'IPDS-II (Stoe)'
_diffrn_measurement_method       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  0.1371
_diffrn_reflns_av_sigmaI/netI    0.2491
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       109
_diffrn_reflns_limit_l_min       -121
_diffrn_reflns_number            59101
_diffrn_reflns_theta_full        25.94
_diffrn_reflns_theta_max         25.94
_diffrn_reflns_theta_min         1.23
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.283
_exptl_absorpt_correction_T_max  0.821
_exptl_absorpt_correction_T_min  0.627
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'Coppens et al. (1965)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             18624
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.305
_refine_diff_density_min         -1.228
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         15185
_refine_ls_number_restraints     62
_refine_ls_restrained_S_all      0.981
_refine_ls_R_factor_all          0.1930
_refine_ls_R_factor_gt           0.0956
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2247
_refine_ls_wR_factor_ref         0.2484
_reflns_number_gt                6064
_reflns_number_total             15185
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901629k_si_004.cif
_cod_data_source_block           2b
_cod_original_cell_volume        35542.5(15)
_cod_original_sg_symbol_H-M      'R -3'
_cod_original_formula_sum        'C254 H253 Ag14 Cl2 O5 P8 Se12.50 Sn'
_cod_database_code               4314443