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_4500172
_publ_contact_author
;

Dr. Rahul Banerjee

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

;
_publ_section_title
;
 Structural and Selective Gas Adsorption Studies of Polyoxometalate and
 Tris(ethylenediamine) Cobalt(III) Based Ionic Crystals
;
_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         'Mo12 O40 P, C6 H24 Co N6, 6(C5 H11 N O) '
_chemical_formula_sum            'C36 H90 Co Mo12 N12 O46 P'
_chemical_formula_weight         2668.38
_chemical_name_common            CoMo12P-DEF
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_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            4
_cell_length_a                   14.395(3)
_cell_length_b                   19.836(4)
_cell_length_c                   28.009(5)
_cell_measurement_reflns_used    4181
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      19.63
_cell_measurement_theta_min      2.27
_cell_volume                     7998(3)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0976
_diffrn_reflns_av_sigmaI/netI    0.1417
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            40586
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.75
_exptl_absorpt_coefficient_mu    2.132
_exptl_absorpt_correction_T_max  0.8151
_exptl_absorpt_correction_T_min  0.6751
_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    2.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Orthorhombic
_exptl_crystal_F_000             5216
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.014
_refine_diff_density_min         -0.789
_refine_diff_density_rms         0.169
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.004(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     788
_refine_ls_number_reflns         14075
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.946
_refine_ls_R_factor_all          0.0886
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1125
_reflns_number_gt                10103
_reflns_number_total             14075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg101201b_si_001.cif
_cod_data_source_block           CoMo12P-DEF
_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 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_database_code               4500172