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_4306114
_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
;
C17 H49 N O8 S7 Y, C16 H48 O8 S8 Y, C4 H12 I16 O2 Pb5 S2
;
_chemical_formula_sum            'C37 H109 I16 N O18 Pb5 S17 Y2'
_chemical_formula_weight         4645.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-10-03
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 98.4301(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0292(2)
_cell_length_b                   15.7685(2)
_cell_length_c                   35.7960(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    150
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     11741.7(2)
_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 0.992
_diffrn_measured_fraction_theta_max 0.984
_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  0.181
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            92074
_diffrn_reflns_theta_full        25.065
_diffrn_reflns_theta_max         27.850
_diffrn_reflns_theta_min         0.979
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    12.670
_exptl_absorpt_correction_T_max  0.08
_exptl_absorpt_correction_T_min  0.01
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             8360
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.59
_refine_diff_density_min         -2.95
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         13994
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.0910
_refine_ls_R_factor_gt           0.0534
_refine_ls_shift/su_max          0.001099
_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: 
 1.55 0.955E-03 1.15 -0.319 0.103 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0736
_refine_ls_wR_factor_gt          0.0608
_refine_ls_wR_factor_ref         0.0572
_reflns_limit_h_max              27
_reflns_limit_h_min              -27
_reflns_limit_k_max              20
_reflns_limit_k_min              0
_reflns_limit_l_max              46
_reflns_limit_l_min              0
_reflns_number_gt                16418
_reflns_number_total             27517
_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   0.0495
_oxford_refine_ls_scale          0.04473(5)
_oxford_reflns_number_all        27421
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'cos in P 21/c'
_cod_data_source_file            ic8010376_si_002_4.cif
_cod_data_source_block           complex_2b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 21/c 1 '
_cod_original_formula_sum        'C37 H109 I16 N1 O18 Pb5 S17 Y2'
_cod_database_code               4306114