Solid-state structural transformations in metal organic-inorganic hybrids constructed from terbium(iii) complexes and iodocuprate clusters
Mishra, Shashank; Jeanneau, Erwann; Ledoux, Gilles; Daniele, Stéphane; CrystEngComm 14 (2012) 3894–; doi:10.1039/c2ce25120e

data_7207994
_publ_section_title
;
 Solid-state structural transformations in metal organic-inorganic hybrids
 constructed from terbium(iii) complexes and iodocuprate clusters
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              3894
_journal_paper_doi               10.1039/c2ce25120e
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C16 H48 O8 S8 Tb, Cu2 I5'
_chemical_formula_sum            'C16 H48 Cu2 I5 O8 S8 Tb'
_chemical_formula_weight         1545.63
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-02-02
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                90
_cell_angle_beta                 91.604(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.1937(5)
_cell_length_b                   9.8578(2)
_cell_length_c                   20.4580(9)
_cell_measurement_reflns_used    3365
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.679
_cell_volume                     2256.56(15)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 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 0.932
_diffrn_measured_fraction_theta_max 0.932
_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  0.035
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7700
_diffrn_reflns_theta_full        27.924
_diffrn_reflns_theta_max         27.924
_diffrn_reflns_theta_min         1.992
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.305
_exptl_absorpt_correction_T_max  0.16
_exptl_absorpt_correction_T_min  0.10
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.494
_exptl_crystal_size_mid          0.326
_exptl_crystal_size_min          0.286
_refine_diff_density_max         2.94
_refine_diff_density_min         -2.51
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9636
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         5023
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0512
_refine_ls_shift/su_max          0.0004823
_refine_ls_shift/su_mean         0.0000242
_refine_ls_structure_factor_coef Fsqd
_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:
31.3 48.5 24.8 6.61
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1631
_refine_ls_wR_factor_gt          0.1348
_refine_ls_wR_factor_ref         0.1631
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              26
_reflns_limit_l_min              0
_reflns_number_gt                3928
_reflns_number_total             5038
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.12
_oxford_diffrn_Wilson_scale      82.99
_oxford_refine_ls_r_factor_ref   0.0669
_oxford_refine_ls_scale          0.11609(7)
_oxford_reflns_number_all        5023
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'scale in P 2/n'
_cod_data_source_file            c2ce25120e.txt
_cod_data_source_block           complex1
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 1 2/n 1 '
_cod_database_code               7207994
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE C ( 7,X'S) H ( 71,X'S) H ( 72,X'S) H ( 73,X'S)
RIDE C ( 3,X'S) H ( 31,X'S) H ( 32,X'S) H ( 33,X'S)
RIDE C ( 4,X'S) H ( 41,X'S) H ( 42,X'S) H ( 43,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S)
RIDE C ( 1,X'S) H ( 11,X'S) H ( 12,X'S) H ( 13,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,X'S)
END
;
_iucr_refine_instruction_details_restraints
;
NO
REM HREST START (DO NOT REMOVE THIS LINE)
REM HREST END (DO NOT REMOVE THIS LINE)
END
;