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_7207996
_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, C2 H6 O S, Cu I3, I '
_chemical_formula_sum            'C18 H54 Cu I4 O9 S9 Tb'
_chemical_formula_weight         1433.30
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             11-01-31
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                86.195(3)
_cell_angle_beta                 87.561(3)
_cell_angle_gamma                87.005(3)
_cell_formula_units_Z            2
_cell_length_a                   10.8626(5)
_cell_length_b                   11.9515(5)
_cell_length_c                   18.3798(8)
_cell_measurement_reflns_used    25304
_cell_measurement_temperature    110
_cell_measurement_theta_max      29.5017
_cell_measurement_theta_min      3.3931
_cell_volume                     2375.80(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_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      110
_diffrn_detector_area_resol_mean 10.4685
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.881
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_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     0.7107
_diffrn_reflns_av_R_equivalents  0.061
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            39872
_diffrn_reflns_theta_full        26.313
_diffrn_reflns_theta_max         29.565
_diffrn_reflns_theta_min         3.400
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.952
_exptl_absorpt_correction_T_max  0.292
_exptl_absorpt_correction_T_min  0.177
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
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            colorless
_exptl_crystal_density_diffrn    2.003
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1368
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.448
_exptl_crystal_size_min          0.353
_refine_diff_density_max         3.10
_refine_diff_density_min         -3.03
_refine_ls_extinction_coef       14.4(13)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0253
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     524
_refine_ls_number_reflns         11729
_refine_ls_number_restraints     298
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.0026053
_refine_ls_shift/su_mean         0.0000747
_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:
0.148E+04 0.226E+04 0.119E+04 332.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1110
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1110
_reflns_limit_h_max              14
_reflns_limit_h_min              -14
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              24
_reflns_limit_l_min              0
_reflns_number_gt                10236
_reflns_number_total             11729
_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   0.0596
_oxford_refine_ls_scale          1.735(7)
_oxford_reflns_number_all        11729
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr265b in P -1'
_cod_data_source_file            c2ce25120e.txt
_cod_data_source_block           complex3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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 '
_cod_original_formula_sum        'C18 H54 Cu1 I4 O9 S9 Tb1'
_cod_database_code               7207996
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 13,X'S) H ( 11,X'S) H ( 12,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 23,X'S) H ( 22,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 ( 43,X'S) H ( 42,X'S) H ( 41,X'S)
RIDE C ( 5,X'S) H ( 51,X'S) H ( 52,X'S) H ( 53,X'S)
RIDE C ( 6,X'S) H ( 61,X'S) H ( 62,X'S) H ( 63,X'S)
RIDE C ( 7,X'S) H ( 73,X'S) H ( 72,X'S) H ( 71,X'S)
RIDE C ( 8,X'S) H ( 82,X'S) H ( 81,X'S) H ( 83,X'S)
RIDE C ( 9,X'S) H ( 93,X'S) H ( 92,X'S) H ( 91,X'S)
RIDE C ( 10,X'S) H ( 101,X'S) H ( 103,X'S) H ( 102,X'S)
RIDE C ( 11,X'S) H ( 111,X'S) H ( 112,X'S) H ( 113,X'S)
RIDE C ( 12,X'S) H ( 121,X'S) H ( 123,X'S) H ( 122,X'S)
RIDE C ( 13,X'S) H ( 132,X'S) H ( 131,X'S) H ( 133,X'S)
RIDE C ( 14,X'S) H ( 141,X'S) H ( 142,X'S) H ( 143,X'S)
RIDE C ( 15,X'S) H ( 152,X'S) H ( 153,X'S) H ( 151,X'S)
RIDE C ( 16,X'S) H ( 163,X'S) H ( 162,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 172,X'S) H ( 173,X'S) H ( 171,X'S)
RIDE C ( 18,X'S) H ( 181,X'S) H ( 182,X'S) H ( 183,X'S)
RIDE C ( 19,X'S) H ( 192,X'S) H ( 191,X'S) H ( 193,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 203,X'S) H ( 202,X'S)
RIDE C ( 21,X'S) H ( 212,X'S) H ( 211,X'S) H ( 213,X'S)
RIDE C ( 22,X'S) H ( 223,X'S) H ( 221,X'S) H ( 222,X'S)
RIDE C ( 23,X'S) H ( 233,X'S) H ( 231,X'S) H ( 232,X'S)
RIDE C ( 24,X'S) H ( 243,X'S) H ( 242,X'S) H ( 241,X'S)
RIDE C ( 25,X'S) H ( 252,X'S) H ( 251,X'S) H ( 253,X'S)
RIDE C ( 26,X'S) H ( 262,X'S) H ( 263,X'S) H ( 261,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)
REM SHIFTLIMIT START (DO NOT REMOVE THIS LINE)
REM SHIFTLIMIT END (DO NOT REMOVE THIS LINE)
U(IJ)'S 0.0, 0.010000 = S(1) TO S(2)
U(IJ)'S 0.0, 0.010000 = S(2) TO S(3)
U(IJ)'S 0.0, 0.010000 = S(3) TO S(4)
U(IJ)'S 0.0, 0.010000 = S(4) TO S(5)
U(IJ)'S 0.0, 0.010000 = S(5) TO S(6)
U(IJ)'S 0.0, 0.010000 = S(6) TO S(7)
U(IJ)'S 0.0, 0.010000 = S(7) TO S(8)
U(IJ)'S 0.0, 0.010000 = S(8) TO S(9)
U(IJ)'S 0.0, 0.010000 = S(9) TO S(10)
U(IJ)'S 0.0, 0.010000 = S(10) TO S(11)
U(IJ)'S 0.0, 0.010000 = S(11) TO S(12)
U(IJ)'S 0.0, 0.010000 = S(12) TO S(13)
U(IJ)'S 0.0, 0.010000 = O(1) TO O(2)
U(IJ)'S 0.0, 0.010000 = O(2) TO O(3)
U(IJ)'S 0.0, 0.010000 = O(3) TO O(4)
U(IJ)'S 0.0, 0.010000 = O(4) TO O(5)
U(IJ)'S 0.0, 0.010000 = O(5) TO O(6)
U(IJ)'S 0.0, 0.010000 = O(6) TO O(7)
U(IJ)'S 0.0, 0.010000 = O(7) TO O(8)
U(IJ)'S 0.0, 0.010000 = O(8) TO O(9)
U(IJ)'S 0.0, 0.010000 = O(9) TO O(10)
U(IJ)'S 0.0, 0.0050000 = O(10) TO O(11)
U(IJ)'S 0.0, 0.0050000 = O(11) TO O(12)
U(IJ)'S 0.0, 0.010000 = O(12) TO O(13)
U(IJ)'S 0.0, 0.010000 = C(1) TO C(2)
U(IJ)'S 0.0, 0.010000 = C(2) TO C(3)
U(IJ)'S 0.0, 0.010000 = C(3) TO C(4)
U(IJ)'S 0.0, 0.010000 = C(4) TO C(5)
U(IJ)'S 0.0, 0.010000 = C(5) TO C(6)
U(IJ)'S 0.0, 0.010000 = C(6) TO C(7)
U(IJ)'S 0.0, 0.010000 = C(7) TO C(8)
U(IJ)'S 0.0, 0.010000 = C(8) TO C(9)
U(IJ)'S 0.0, 0.010000 = C(9) TO C(10)
U(IJ)'S 0.0, 0.010000 = C(10) TO C(11)
U(IJ)'S 0.0, 0.010000 = C(11) TO C(12)
U(IJ)'S 0.0, 0.010000 = C(12) TO C(13)
U(IJ)'S 0.0, 0.010000 = C(13) TO C(14)
U(IJ)'S 0.0, 0.010000 = C(14) TO C(15)
U(IJ)'S 0.0, 0.010000 = C(15) TO C(16)
U(IJ)'S 0.0, 0.010000 = C(16) TO C(17)
U(IJ)'S 0.0, 0.010000 = C(17) TO C(18)
U(IJ)'S 0.0, 0.010000 = C(18) TO C(19)
U(IJ)'S 0.0, 0.010000 = C(19) TO C(20)
U(IJ)'S 0.0, 0.010000 = C(20) TO C(21)
U(IJ)'S 0.0, 0.010000 = C(21) TO C(22)
U(IJ)'S 0.0, 0.010000 = C(22) TO C(23)
U(IJ)'S 0.0, 0.010000 = C(23) TO C(24)
U(IJ)'S 0.0, 0.010000 = C(24) TO C(25)
U(IJ)'S 0.0, 0.010000 = C(25) TO C(26)
DISTANCE 1.800000 , 0.0050000 = C(18) TO S(9)
DISTANCE 1.800000 , 0.0050000 = C(10) TO S(5)
DISTANCE 1.800000 , 0.0050000 = C(23) TO S(12)
DISTANCE 1.800000 , 0.0050000 = C(16) TO S(8)
END
;