Synthesis and Phase Width of Quaternary Selenides Pb4InxM6-xSe13 (M = Bi,x= 2.1-2.8; Sb,x= 2)
Chi-Shen Lee; Ming-Fang Wang; Wen-Hen Huang; Inorganic Chemistry 48 (2009) 6402–6408; doi:10.1021/ic8023875

data_4302602
_publ_contact_author_address
;Department of Applied Chemistry
National Chiao Tung University
1001 University Rd, Hsinchu, 30010, Taiwan
;
_publ_contact_author_email       chishen@mail.nctu.edu.tw
_publ_contact_author_fax         1-886-3-5723764
_publ_contact_author_name        'Chi-Shen Lee'
_publ_contact_author_phone       1-886-3-5131332
_publ_section_title
;
Synthesis and Phase Width of Quaternary Selenides Pb4InxM6-xSe13 (M =
Bi,x= 2.1-2.8; Sb,x= 2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6402
_journal_page_last               6408
_journal_paper_doi               10.1021/ic8023875
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         Pb4In2.1Bi3.9Se13
_chemical_formula_sum            'Bi3.9 In2.1 Pb4 Se13'
_chemical_formula_weight         2911.42
_chemical_name_systematic        'bismuth indium lead selenide(3.9/2.1/4/13)'
_space_group_IT_number           55
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      55
_symmetry_space_group_name_Hall  '-P 2 2ab'
_symmetry_space_group_name_H-M   'P b a m'
_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                   22.273(5)
_cell_length_b                   27.488(6)
_cell_length_c                   4.1418(8)
_cell_measurement_reflns_used    29610
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      1.18
_cell_volume                     2535.8(9)
_computing_cell_refinement       'Bruker Smart Apex'
_computing_data_collection       'Bruker Smart Apex'
_computing_data_reduction        'Bruker Smart Apex'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0586
_diffrn_reflns_av_sigmaI/netI    0.0377
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            29610
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         1.18
_diffrn_source                   'fine-focus sealed tube'
_diffrn_source_type              'Bruker Apex CCD'
_exptl_absorpt_coefficient_mu    73.930
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.267146
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
 The absorption correction was based on 7171 symmetry-equivalent reflections
 using the SADABS program. Sheldric, G. M. (1996). SADABS. Bruker Area Detector 
 Absorption Correction Software. University of Gottingen, Germany. 
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    7.626
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             4786.7
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.966
_refine_diff_density_min         -3.614
_refine_diff_density_rms         0.444
_refine_ls_extinction_coef       0.000121(11)
_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   1.168
_refine_ls_matrix_type           full
_refine_ls_number_parameters     148
_refine_ls_number_reflns         3603
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.168
_refine_ls_R_factor_all          0.0398
_refine_ls_R_factor_gt           0.0315
_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^)+(0.0265P)^2^+5.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0676
_refine_ls_wR_factor_ref         0.0700
_reflns_number_gt                3112
_reflns_number_total             3603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic8023875_si_002_2.cif
_cod_data_source_block           Pb4In2.1Bi3.9Se13
_cod_depositor_comments
;
The following automatic conversions were performed:
'_geom_bond_publ_flag' value 'Yes' changed to 'yes' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (62
times).

'_geom_bond_publ_flag' value 'No' changed to 'no' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (48
times).

'_geom_angle_publ_flag' value 'No' changed to 'no' 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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4302602