Structural and Selective Gas Adsorption Studies of Polyoxometalate and Tris(ethylenediamine) Cobalt(III) Based Ionic Crystals
Dey, Chandan; Das, Raja; Pachfule, Pradip; Poddar, Pankaj; Banerjee, Rahul; Crystal Growth & Design 11 (2011) 139–; doi:10.1021/cg101201b

data_4500177
_publ_contact_author
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Dr. Rahul Banerjee

Scientist
Physical/Materials Chemistry Division  
National Chemical Laboratory
Dr. Homi Bhaba Road
Pune 411008, India

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_publ_section_title
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 Structural and Selective Gas Adsorption Studies of Polyoxometalate and
 Tris(ethylenediamine) Cobalt(III) Based Ionic Crystals
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_journal_issue                   1
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              139
_journal_paper_doi               10.1021/cg101201b
_journal_volume                  11
_journal_year                    2011
_chemical_formula_moiety
'2(O40SiW12),3(C6H24CoN6), 12(C3H7NO),Cl,3(O)'
_chemical_formula_sum            'C54 H156 Cl Co3 N30 O95 Si2 W24'
_chemical_formula_weight         7426.67
_chemical_name_common            CoW12Si-DMF
_chemical_name_systematic
; 
 ? 
;
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.3400(10)
_cell_angle_beta                 95.4740(10)
_cell_angle_gamma                97.373(2)
_cell_formula_units_Z            2
_cell_length_a                   13.1948(11)
_cell_length_b                   20.9672(18)
_cell_length_c                   29.020(3)
_cell_measurement_reflns_used    6109
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.83
_cell_measurement_theta_min      2.47
_cell_volume                     7905.7(13)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SMART'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1000
_diffrn_reflns_av_sigmaI/netI    0.1012
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            77225
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    17.813
_exptl_absorpt_correction_T_max  0.9653
_exptl_absorpt_correction_T_min  0.9486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-58'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    3.120
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             6704
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         5.911
_refine_diff_density_min         -4.148
_refine_diff_density_rms         0.583
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1436
_refine_ls_number_reflns         27818
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0933
_refine_ls_R_factor_gt           0.0782
_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^)+(0.1009P)^2^+53.7690P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2046
_refine_ls_wR_factor_ref         0.2179
_reflns_number_gt                21997
_reflns_number_total             27818
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101201b_si_001.cif
_cod_data_source_block           CoW12Si-DMF
_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        7905.6(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4500177