Solid- and Solution Phase Transformations in Novel Hybrid Iodoplumbate Derivatives Templated by Solvated Yttrium Complexes
Shashank Mishra; Erwann Jeanneau; Stéphane Daniele; Gilles Ledoux; Prakash N. Swamy; Inorganic Chemistry 47 (2008) 9333–9343; doi:10.1021/ic8010376

data_4306111
_publ_contact_author_address
;Universit\'e Claude Bernard Lyon 1
IRCELYON
2 avenue A. Einstein
69626 Villeurbanne C\'edex
France.
;
_publ_contact_author_email       mishrashashank74@rediffmail.com
_publ_contact_author_fax         '(+33) 472445399'
_publ_contact_author_name        'Dr. Shashank Mishra'
_publ_contact_author_phone       '(+33) 472445329'
_publ_section_title
;
Solid- and Solution Phase Transformations in Novel Hybrid Iodoplumbate
Derivatives Templated by Solvated Yttrium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9333
_journal_page_last               9343
_journal_paper_doi               10.1021/ic8010376
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'I18 Pb6, 2(C14 H42 O7 S7 Y)'
_chemical_formula_sum            'C28 H84 I18 O14 Pb6 S14 Y2'
_chemical_formula_weight         4799.18
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-10-02
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                95.739(2)
_cell_angle_beta                 94.6285(17)
_cell_angle_gamma                93.4272(19)
_cell_formula_units_Z            2
_cell_length_a                   15.2810(5)
_cell_length_b                   17.5643(5)
_cell_length_c                   19.4559(7)
_cell_measurement_reflns_used    96250
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     5166.7(3)
_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 0.988
_diffrn_measured_fraction_theta_max 0.964
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43371
_diffrn_reflns_theta_full        25.134
_diffrn_reflns_theta_max         27.927
_diffrn_reflns_theta_min         1.168
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.545
_exptl_absorpt_correction_T_max  0.12
_exptl_absorpt_correction_T_min  0.04
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    3.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4224
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.13
_refine_diff_density_max         2.20
_refine_diff_density_min         -2.05
_refine_ls_extinction_coef       1.879
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     739
_refine_ls_number_reflns         16388
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002821
_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: 
 0.726 0.580 0.367 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0944
_refine_ls_wR_factor_gt          0.0515
_refine_ls_wR_factor_ref         0.0515
_reflns_limit_h_max              19
_reflns_limit_h_min              -20
_reflns_limit_k_max              22
_reflns_limit_k_min              -23
_reflns_limit_l_max              25
_reflns_limit_l_min              0
_reflns_number_gt                16388
_reflns_number_total             23906
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.18
_oxford_diffrn_Wilson_scale      402.81
_oxford_refine_ls_r_factor_ref   0.0446
_oxford_refine_ls_scale          0.04953(5)
_oxford_reflns_number_all        23824
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_oxford_structure_analysis_title 'import in P -1'
_cod_data_source_file            ic8010376_si_002_1.cif
_cod_data_source_block           complex_4
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      'P -1 '
_cod_database_code               4306111