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_7207995
_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         'C24 H56 N8 O8 Tb, Cu I3, I'
_chemical_formula_sum            'C24 H56 Cu I4 N8 O8 Tb'
_chemical_formula_weight         1314.85
_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             11-02-02
_audit_creation_method           CRYSTALS_ver_14.11
_cell_angle_alpha                79.5186(11)
_cell_angle_beta                 73.0295(11)
_cell_angle_gamma                73.5139(10)
_cell_formula_units_Z            2
_cell_length_a                   11.00230(20)
_cell_length_b                   12.94800(20)
_cell_length_c                   17.05820(29)
_cell_measurement_reflns_used    26873
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.878
_cell_measurement_theta_min      0.679
_cell_volume                     2215.66(7)
_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 0.995
_diffrn_measured_fraction_theta_max 0.992
_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  0.022
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19410
_diffrn_reflns_theta_full        25.600
_diffrn_reflns_theta_max         27.826
_diffrn_reflns_theta_min         1.255
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.895
_exptl_absorpt_correction_T_max  0.3406
_exptl_absorpt_correction_T_min  0.2856
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1252
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.220
_refine_diff_density_max         1.08
_refine_diff_density_min         -1.32
_refine_ls_extinction_coef       64(2)
_refine_ls_extinction_method     'Larson (1970), Equation 22'
_refine_ls_goodness_of_fit_ref   0.9046
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         10392
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.0015852
_refine_ls_shift/su_mean         0.0000247
_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:
7.42 9.48 3.18
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0748
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0748
_reflns_limit_h_max              14
_reflns_limit_h_min              -13
_reflns_limit_k_max              16
_reflns_limit_k_min              -16
_reflns_limit_l_max              22
_reflns_limit_l_min              0
_reflns_number_gt                8802
_reflns_number_total             10429
_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   0.0387
_oxford_refine_ls_scale          0.14606(4)
_oxford_reflns_number_all        10392
_oxford_reflns_threshold_expression_ref I>-10.0\s(I)
_oxford_structure_analysis_title 'scale in P -1'
_cod_data_source_file            c2ce25120e.txt
_cod_data_source_block           complex2
_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_cell_volume        2215.657(67)
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C24 H56 Cu1 I4 N8 O8 Tb1'
_cod_database_code               7207995
_iucr_refine_instruction_details_constraints
;
BLOCK SCALE X'S, U'S
CONT EXTPARAM
RIDE C ( 1,X'S) H ( 11,X'S)
RIDE C ( 2,X'S) H ( 21,X'S) H ( 22,X'S) H ( 23,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)
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 ( 71,X'S)
RIDE C ( 8,X'S) H ( 81,X'S) H ( 82,X'S) H ( 83,X'S)
RIDE C ( 9,X'S) H ( 91,X'S) H ( 92,X'S) H ( 93,X'S)
RIDE C ( 10,X'S) H ( 101,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 ( 122,X'S) H ( 123,X'S)
RIDE C ( 13,X'S) H ( 131,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 ( 151,X'S) H ( 152,X'S) H ( 153,X'S)
RIDE C ( 16,X'S) H ( 161,X'S)
RIDE C ( 17,X'S) H ( 171,X'S) H ( 172,X'S) H ( 173,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 ( 191,X'S)
RIDE C ( 20,X'S) H ( 201,X'S) H ( 202,X'S) H ( 203,X'S)
RIDE C ( 21,X'S) H ( 211,X'S) H ( 212,X'S) H ( 213,X'S)
RIDE C ( 22,X'S) H ( 221,X'S)
RIDE C ( 23,X'S) H ( 231,X'S) H ( 232,X'S) H ( 233,X'S)
RIDE C ( 24,X'S) H ( 241,X'S) H ( 242,X'S) H ( 243,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
;