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_7207997
_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, I3, 2(I)'
_chemical_formula_sum            'C16 H48 I5 O8 S8 Tb'
_chemical_formula_weight         1418.53
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2b'
_symmetry_space_group_name_H-M   'P b n a'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.4740(10)
_cell_length_b                   18.5970(10)
_cell_length_c                   12.222(2)
_cell_measurement_reflns_used    6773
_cell_measurement_temperature    110
_cell_measurement_theta_max      30.0387
_cell_measurement_theta_min      3.4453
_cell_volume                     4426.3(8)
_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 0.996
_diffrn_measured_fraction_theta_max 0.851
_diffrn_measurement_device_type  'Xcalibur, Atlas, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_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  0.055
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            15199
_diffrn_reflns_theta_full        26.309
_diffrn_reflns_theta_max         29.560
_diffrn_reflns_theta_min         3.458
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.493
_exptl_absorpt_correction_T_max  0.374
_exptl_absorpt_correction_T_min  0.215
_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            purple
_exptl_crystal_density_diffrn    2.129
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2664
_exptl_crystal_size_max          0.481
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.266
_refine_diff_density_max         4.81
_refine_diff_density_min         -6.49
_refine_ls_extinction_coef       37(3)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   1.0551
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         5276
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1141
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.0003862
_refine_ls_shift/su_mean         0.0000249
_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:
0.295E+04 0.377E+04 0.217E+04 678. 93.9
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1739
_refine_ls_wR_factor_gt          0.1689
_refine_ls_wR_factor_ref         0.1739
_reflns_limit_h_max              26
_reflns_limit_h_min              0
_reflns_limit_k_max              25
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                4493
_reflns_number_total             5276
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   2.10
_oxford_diffrn_Wilson_scale      0.25
_oxford_refine_ls_r_factor_ref   0.1141
_oxford_refine_ls_scale          1.194(8)
_oxford_reflns_number_all        5276
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'smr265a in P m n a'
_cod_data_source_file            c2ce25120e.txt
_cod_data_source_block           complex4
_cod_original_sg_symbol_H-M      'P b n a '
_cod_database_code               7207997
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 6,X'S) H ( 63,X'S) H ( 62,X'S) H ( 61,X'S)
RIDE C ( 5,X'S) H ( 53,X'S) H ( 52,X'S) H ( 51,X'S)
RIDE C ( 8,X'S) H ( 83,X'S) H ( 82,X'S) H ( 81,X'S)
RIDE C ( 7,X'S) H ( 73,X'S) H ( 72,X'S) H ( 71,X'S)
RIDE C ( 4,X'S) H ( 43,X'S) H ( 42,X'S) H ( 41,X'S)
RIDE C ( 3,X'S) H ( 33,X'S) H ( 32,X'S) H ( 31,X'S)
RIDE C ( 2,X'S) H ( 23,X'S) H ( 22,X'S) H ( 21,X'S)
RIDE C ( 1,X'S) H ( 13,X'S) H ( 12,X'S) H ( 11,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)
U(IJ)'S 0.0, 0.010000 = C(6) TO C(5)
END
;