Disassembly and Reassembly of Polyoxometalates: The Formation of Chains from an Adaptable Precursor
Ritchie, Chris; Boskovic, Colette; Crystal Growth & Design 10 (2010) 488–; doi:10.1021/cg901400k

data_4502575
_publ_section_title
;
 Disassembly and Reassembly of Polyoxometalates: The Formation of Chains
 from an Adaptable Precursor
;
_journal_issue                   2
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              488
_journal_paper_doi               10.1021/cg901400k
_journal_volume                  10
_journal_year                    2010
_chemical_formula_moiety
'K2, Na2, (H96 Dy8 As4 W44 O198 C8 N4), 41(H2O) '
_chemical_formula_sum            'C8 H178 As4 Dy8 K2 N4 Na2 O239 W44'
_chemical_formula_weight         13968.21
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.1515(2)
_cell_length_b                   19.8626(2)
_cell_length_c                   24.6483(2)
_cell_measurement_reflns_used    12915
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      50.9859
_cell_measurement_theta_min      2.6796
_cell_volume                     10844.92(17)
_computing_cell_refinement
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_data_collection
; 
CrysAlis CCD, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_data_reduction
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_detector_area_resol_mean 16.0711
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'XCalibur S CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0419
_diffrn_reflns_av_sigmaI/netI    0.0381
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20394
_diffrn_reflns_theta_full        50.99
_diffrn_reflns_theta_max         50.99
_diffrn_reflns_theta_min         2.68
_exptl_absorpt_coefficient_mu    58.481
_exptl_absorpt_correction_T_max  0.472
_exptl_absorpt_correction_T_min  0.058
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlis RED, Oxford Diffraction Ltd., 
Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) 
(compiled Jan 10 2008,16:37:18) 
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            Colourless
_exptl_crystal_density_diffrn    4.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             11928
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.047
_exptl_crystal_size_min          0.028
_refine_diff_density_max         3.372
_refine_diff_density_min         -1.747
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     543
_refine_ls_number_reflns         5994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+25.4667P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1051
_refine_ls_wR_factor_ref         0.1079
_reflns_number_gt                5069
_reflns_number_total             5994
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg901400k_si_001.cif
_cod_data_source_block           cr112e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_original_formula_sum        'As4 C8 Dy8 H178 K2 N4 Na2 O239 W44'
_cod_database_code               4502575