Lanthanide complexes in hybrid halometallate materials: interconversion between a novel 2D microporous framework and a 1D zigzag chain structure of iodoargentates templated by octakis-solvated terbium(III) cation
Mishra, Shashank; Jeanneau, Erwann; Ledoux, Gilles; Daniele, Stéphane; Dalton Transactions  (2009) 4954–4961; doi:10.1039/b903576a

data_7001490
_publ_section_title
;
 Lanthanide complexes in hybrid halometallate materials:
 interconversion between a novel 2D microporous framework and a 1D
 zigzag chain structure of iodoargentates templated by octakis-solvated
 terbium(III) cation
;
_journal_issue                   25
_journal_name_full               'Dalton Transactions'
_journal_page_first              4954
_journal_page_last               4961
_journal_paper_doi               10.1039/b903576a
_journal_year                    2009
_chemical_formula_moiety         'C16 H48 I3 O8 S8 Tb1'
_chemical_formula_sum            'C16 H48 I3 O8 S8 Tb'
_chemical_formula_weight         1164.72
_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             08-12-11
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.6061(12)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            4
_cell_length_a                   12.39430(20)
_cell_length_b                   18.69510(40)
_cell_length_c                   17.68630(29)
_cell_measurement_reflns_used    35123
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.730
_cell_volume                     4040.68(13)
_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 0.981
_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  0.021
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17321
_diffrn_reflns_theta_full        25.099
_diffrn_reflns_theta_max         27.888
_diffrn_reflns_theta_min         1.597
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.487
_exptl_absorpt_correction_T_max  0.1818
_exptl_absorpt_correction_T_min  0.1519
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.915
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.38
_refine_diff_density_max         3.04
_refine_diff_density_min         -3.06
_refine_ls_extinction_coef       67(8)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0584
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     326
_refine_ls_number_reflns         8085
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0419
_refine_ls_shift/su_max          0.001107
_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:
1.24 0.357 0.768
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0477
_refine_ls_wR_factor_gt          0.0450
_refine_ls_wR_factor_ref         0.0448
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              24
_reflns_limit_k_min              0
_reflns_limit_l_max              23
_reflns_limit_l_min              0
_reflns_number_gt                8391
_reflns_number_total             9469
_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   0.0402
_oxford_refine_ls_scale          0.2015(3)
_oxford_reflns_number_all        9440
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'scale in P 21/n'
_cod_data_source_file            b903576a.txt
_cod_data_source_block           complex_1
_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        4040.677(128)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_original_formula_sum        'C16 H48 I3 O8 S8 Tb1'
_cod_database_code               7001490