Solvothermal synthesis of a new 3-D mixed-metal sulfide framework, (H1.33tren)[In2.67Sb1.33S8]·tren
Lampkin, John D.; Powell, Anthony V.; Chippindale, Ann M.; Journal of Solid State Chemistry 243 (2016) 44–49; doi:10.1016/j.jssc.2016.08.007

data_1561333
_publ_section_title
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 Solvothermal synthesis of a new 3-D mixed-metal sulfide framework,
 (H1.33tren)[In2.67Sb1.33S8]&#x00B7;tren
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_journal_name_full               'Journal of Solid State Chemistry'
_journal_page_first              44
_journal_page_last               49
_journal_paper_doi               10.1016/j.jssc.2016.08.007
_journal_volume                  243
_journal_year                    2016
_chemical_absolute_configuration .
_chemical_formula_moiety         'In2.67 S8 Sb1.33'
_chemical_formula_sum            'In2.67 S8 Sb1.33'
_chemical_formula_weight         725.025
_space_group_IT_number           122
_space_group_name_Hall           'I -4 2bw'
_space_group_name_H-M_alt        'I -4 2 d'
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I -4 2bw'
_symmetry_space_group_name_H-M   'I -4 2 d'
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.6248(5)
_cell_length_b                   12.6248(5)
_cell_length_c                   19.4387(18)
_cell_measurement_reflns_used    1044
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.135
_cell_measurement_theta_min      3.098
_cell_volume                     3098.2(3)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'Gemini, (Oxford Diffraction, 2006)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction Gemini'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.028
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1044
_diffrn_reflns_theta_full        25.056
_diffrn_reflns_theta_max         29.135
_diffrn_reflns_theta_min         3.098
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         .
_exptl_absorpt_coefficient_mu    3.627
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.69
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrysAlis, (Oxford Diffraction, 2002)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1307.660
_exptl_crystal_size_max          0.103
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.087
_refine_diff_density_max         1.37
_refine_diff_density_min         -0.71
_refine_ls_abs_structure_details 'Flack (1983), 0 Friedel-pairs'
_refine_ls_abs_structure_Flack   -0.16(3)
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9974
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     29
_refine_ls_number_reflns         828
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0608
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.0055399
_refine_ls_shift/su_mean         0.0015489
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] 
 where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ 
 A~i~ are: 
 5.73 -0.914 4.27 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0604
_refine_ls_wR_factor_gt          0.0565
_refine_ls_wR_factor_ref         0.0552
_reflns_limit_h_max              12
_reflns_limit_h_min              0
_reflns_limit_k_max              17
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                897
_reflns_number_total             1044
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_r_factor_ref   0.0519
_oxford_refine_ls_scale          0.611(3)
_oxford_reflns_number_all        1039
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            JSSC-2016-243-44.cif
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      'I -4 2 d '
_cod_database_code               1561333
_iucr_refine_instructions_details_constraints
;
FULL IN(1, X'S, U'S) UNTIL LAST 
RIDE SB(1, X'S, U'S) IN(1, X'S, U'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
NO 
END                                                                             
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