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_7207998
_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_absolute_configuration ad
_chemical_formula_moiety         'C18 H48 N6 O9 Tb, Cu9 I14 '
_chemical_formula_sum            'C18 H48 Cu9 I14 N6 O9 Tb'
_chemical_formula_weight         3000.10
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             09-03-18
_audit_creation_method           CRYSTALS_ver_12.86
_cell_angle_alpha                90.0
_cell_angle_beta                 90.0
_cell_angle_gamma                120.0
_cell_formula_units_Z            6
_cell_length_a                   13.83(2)
_cell_length_b                   13.83(2)
_cell_length_c                   61.5(4)
_cell_measurement_reflns_used    184
_cell_measurement_temperature    150
_cell_measurement_theta_max      29.4426
_cell_measurement_theta_min      3.1034
_cell_volume                     10187(7)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
;
_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_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.895
_diffrn_measurement_device       'Oxford Diffraction XCALIBUR'
_diffrn_measurement_device_type
;
Goniometer Xcalibur, detector: Atlas (Gemini ultra Mo)
;
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.060
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       84
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2838
_diffrn_reflns_theta_full        26.582
_diffrn_reflns_theta_max         29.535
_diffrn_reflns_theta_min         3.109
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    10.183
_exptl_absorpt_correction_T_max  0.22
_exptl_absorpt_correction_T_min  0.15
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.934
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             8028
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
;
_refine_diff_density_max         2.39
_refine_diff_density_min         -1.08
_refine_ls_abs_structure_details 'Flack (1983), 2197 Friedel-pairs'
_refine_ls_extinction_coef       80(10)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0930
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     91
_refine_ls_number_reflns         1305
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0632
_refine_ls_shift/su_max          0.004177
_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:
10.8 0.675 5.74
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1363
_refine_ls_wR_factor_gt          0.0709
_refine_ls_wR_factor_ref         0.0671
_reflns_limit_h_max              0
_reflns_limit_h_min              -16
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              84
_reflns_limit_l_min              0
_reflns_number_gt                1457
_reflns_number_total             2838
_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   0.0583
_oxford_refine_ls_scale          0.490(3)
_oxford_reflns_number_all        2831
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'SMR147b in R-3c'
_cod_data_source_file            c2ce25120e.txt
_cod_data_source_block           complex5
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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_cell_volume        10187(84)
_cod_original_sg_symbol_Hall     '-R 3 2"c '
_cod_original_sg_symbol_H-M      'R -3 c '
_cod_database_code               7207998