Layered Cobalt Hydroxysulfates with Both Rigid and Flexible Organic Pillars: Synthesis, Structure, Porosity, and Cooperative Magnetism
Apinpus Rujiwatra; Cameron J. Kepert; John B. Claridge; Matthew J. Rosseinsky; Hitoshi Kumagai; Mohamedally Kurmoo; Journal of the American Chemical Society 123 (2001) 10584–10594; doi:10.1021/ja0109848

data_4115743
_publ_contact_author
;

      Matthew J. Rosseinsky

      Department of Chemistry
      University of Liverpool 
      Liverpool L69 7ZD
      UK
;
_publ_contact_author_email       m.j.rosseinsky@liverpool.ac.uk
_publ_contact_author_fax         '(44) 151 7943587'
_publ_contact_author_phone       '(44) 151 7943499'
_publ_section_title
;
 Layered Cobalt Hydroxysulfates with Both Rigid and Flexible Organic
 Pillars: Synthesis, Structure, Porosity, and Cooperative Magnetism
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10584
_journal_page_last               10594
_journal_paper_doi               10.1021/ja0109848
_journal_volume                  123
_journal_year                    2001
_chemical_compound_source
;
 'hydrothermal synthesis at 180 deg C for 3 days'
;
_chemical_formula_moiety         'C H10 Co4 N O10 S, 3(H2 O)'
_chemical_formula_sum            'C H16 Co4 N O13 S'
_chemical_formula_weight         517.93
_chemical_name_common            csen
_chemical_name_systematic
; 
 mu-ethylenediaminododecahydroxodisulfatooctacobalt(II)-6-water 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      147
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            2
_cell_length_a                   8.298(1)
_cell_length_b                   8.298(1)
_cell_length_c                   10.519(2)
_cell_measurement_reflns_used    11099
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.58
_cell_measurement_theta_min      2.83
_cell_volume                     627.27(16)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'RC93 (Watkin et al., 1994)'
_computing_molecular_graphics    XPMA/ZORTEP
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_environment
;
 'In thin film of perfluorpolyether oil on mohair fibre'
;
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment        'Flash cooled in nitrogen stream'
_diffrn_detector                 'Eu/Ba image plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device       'Enraf-Nonius DIP2000 diffractometer'
_diffrn_measurement_method       'Ninety 2-degree oscillations in phi'
_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  0.054
_diffrn_reflns_av_sigmaI/netI    0.0265
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3396
_diffrn_reflns_theta_full        26.58
_diffrn_reflns_theta_max         26.58
_diffrn_reflns_theta_min         2.83
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    5.432
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  1.0
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.742
_exptl_crystal_description       'transparent platelets'
_exptl_crystal_F_000             514
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.938
_refine_diff_density_min         -1.332
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.321
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     64
_refine_ls_number_reflns         875
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.320
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0859
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^+12.8917P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2179
_refine_ls_wR_factor_ref         0.2193
_reflns_number_gt                839
_reflns_number_total             875
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0109848_2.cif
_cod_data_source_block           Co8(SO4)2(OH)12(en).6(H2O)
_cod_original_cell_volume        627.3(2)
_cod_database_code               4115743