Rare example of a polynuclear heterometallic yttrium(III)‒copper(I) iodide cluster with a [Y6(μ6-O)(μ3-OH)8]8+ core structure showing single crystal-to-single crystal transformation
Mishra, Shashank; Jeanneau, Erwann; Daniele, Stéphane; Hubert-Pfalzgraf, Liliane G.; CrystEngComm 10 (2008) 814–; doi:10.1039/b802434k

data_7202010
_publ_section_title
;
 Rare example of a polynuclear heterometallic yttrium(III)--copper(I)
 iodide cluster with a [Y6(\m6-O)(\m3-OH)8]8+ core structure showing
 single crystal-to-single crystal transformation
;
_journal_issue                   7
_journal_name_full               CrystEngComm
_journal_page_first              814
_journal_paper_doi               10.1039/b802434k
_journal_volume                  10
_journal_year                    2008
_chemical_formula_moiety
;
C32 H104 O27 S16 Y6, Cu2 I4, 6(I)
;
_chemical_formula_sum            'C32 H104 Cu2 I10 O27 S16 Y6'
_chemical_formula_weight         3363.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-10-03
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90.0000
_cell_angle_beta                 91.0374(35)
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   14.29910(100)
_cell_length_b                   19.29990(150)
_cell_length_c                   18.79500(119)
_cell_measurement_reflns_used    51056
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.534
_cell_measurement_theta_min      0.730
_cell_volume                     5186.0(6)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_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 0.996
_diffrn_measured_fraction_theta_max 0.995
_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  0.041
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13386
_diffrn_reflns_theta_full        23.075
_diffrn_reflns_theta_max         23.545
_diffrn_reflns_theta_min         2.091
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.069
_exptl_absorpt_correction_T_max  0.79
_exptl_absorpt_correction_T_min  0.59
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
Analytical Absorption (De Meulenaer & Tompa, 1965)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.154
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3180
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         2.57
_refine_diff_density_min         -1.94
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.2006
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         3432
_refine_ls_number_restraints     174
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0885
_refine_ls_shift/su_max          0.000443
_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:
1.64 1.43 1.19
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1139
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0864
_reflns_limit_h_max              16
_reflns_limit_h_min              -16
_reflns_limit_k_max              21
_reflns_limit_k_min              0
_reflns_limit_l_max              21
_reflns_limit_l_min              0
_reflns_number_gt                4045
_reflns_number_total             7670
_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   0.0809
_oxford_refine_ls_scale          0.0710(3)
_oxford_reflns_number_all        7643
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_oxford_structure_analysis_title 'scale in P 21/n'
_cod_data_source_file            b802434k.txt
_cod_data_source_block           complex_1
_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_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        5186.029(635)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7202010