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_4306115
_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         '    C18 H42 N6 O8 Y, I9 Pb3'
_chemical_formula_sum            'C18 H42 I9 N6 O8 Pb3 Y'
_chemical_formula_weight         2323.21
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-06-13
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.737(3)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   10.4355(5)
_cell_length_b                   18.4559(9)
_cell_length_c                   27.2727(7)
_cell_measurement_reflns_used    8751
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.713
_cell_measurement_theta_min      0.848
_cell_volume                     5160.7(4)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD'
_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  0.086
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            17056
_diffrn_reflns_theta_full        24.703
_diffrn_reflns_theta_max         24.703
_diffrn_reflns_theta_min         1.340
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    16.290
_exptl_absorpt_correction_T_max  0.61
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
 Analytical Absorption (De Meulenaer & Tompa, 1965) 
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.990
_exptl_crystal_description       needle
_exptl_crystal_F_000             4072
_exptl_crystal_size_max          0.07
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.06
_refine_diff_density_min         -2.09
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     409
_refine_ls_number_reflns         4161
_refine_ls_number_restraints     108
_refine_ls_R_factor_all          0.1239
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.000317
_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: 
 0.313 0.240 0.132 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1287
_refine_ls_wR_factor_gt          0.0548
_refine_ls_wR_factor_ref         0.0548
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              32
_reflns_limit_l_min              0
_reflns_number_gt                4161
_reflns_number_total             8761
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   0.00
_oxford_diffrn_Wilson_scale      0.00
_oxford_refine_ls_scale          0.01483(3)
_oxford_structure_analysis_title 'import in P 21/n'
_cod_data_source_file            ic8010376_si_002_5.cif
_cod_data_source_block           complex_3
_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_cell_volume        5160.66(38)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C18 H42 I9 N6 O8 Pb3 Y1'
_cod_database_code               4306115