Reactions of metal iodides as a simple route to heterometallics: synthesis, structural transformations, thermal and luminescent properties of novel hybrid iodoargentate derivatives templated by [YL8]3+ or [YL7]3+ cations (L = DMF or DMSO)
Mishra, Shashank; Jeanneau, Erwann; Daniele, Stéphane; Ledoux, Gilles; Dalton Transactions  (2008) 6296–6304; doi:10.1039/B809964B

data_7004666
_publ_section_title
;
 Reactions of metal iodides as a simple route to heterometallics:
 synthesis, structural transformations, thermal and luminescent
 properties of novel hybrid iodoargentate derivatives templated by
 [YL8]3+ or [YL7]3+ cations (L = DMF or DMSO)
;
_journal_issue                   44
_journal_name_full               'Dalton Transactions'
_journal_page_first              6296
_journal_page_last               6304
_journal_paper_doi               10.1039/B809964B
_journal_year                    2008
_chemical_absolute_configuration unk
_chemical_formula_moiety         'C112 H330.00 Ag24 I48 O56.00 S56.00 Y8.00'
_chemical_formula_sum            'C112 H330 Ag24 I48 O56 S56 Y8'
_chemical_formula_weight         13761.00
_space_group_IT_number           146
_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
_audit_creation_date             08-05-28
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   40.194(2)
_cell_length_b                   40.194(2)
_cell_length_c                   19.195(3)
_cell_measurement_reflns_used    7142
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     26856(5)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.832
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.098
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       45
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30244
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         27.888
_diffrn_reflns_theta_min         1.211
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.069
_exptl_absorpt_correction_T_max  0.32
_exptl_absorpt_correction_T_min  0.23
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Siemens, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             18989.994
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_refine_diff_density_max         3.32
_refine_diff_density_min         -1.88
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1494
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         7142
_refine_ls_number_restraints     474
_refine_ls_R_factor_all          0.1683
_refine_ls_R_factor_gt           0.0725
_refine_ls_shift/su_max          0.004767
_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:
1.11 0.275 0.553
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1896
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0648
_reflns_limit_h_max              24
_reflns_limit_h_min              -49
_reflns_limit_k_max              48
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              -25
_reflns_number_gt                8483
_reflns_number_total             16985
_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   0.0601
_oxford_refine_ls_scale          0.02048(3)
_oxford_reflns_number_all        16906
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'sadabs in R -3'
_cod_data_source_file            B809964B.txt
_cod_data_source_block           complex_5
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal' 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_original_sg_symbol_H-M      'R 3 '
_cod_original_formula_sum        'C112 H330.00 Ag24 I48 O56.00 S56.00 Y8.00'
_cod_database_code               7004666