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_4115742
_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 200 deg C for 30 hours'
;
_chemical_formula_moiety         'C3 H12 Co4 N O10 S,(H2O)'
_chemical_formula_sum            'C3 H14 Co4 N O11 S'
_chemical_formula_weight         507.94
_chemical_name_common            csdab
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           165
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3 2"c'
_symmetry_space_group_name_H-M   'P -3 c 1'
_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            3
_cell_length_a                   8.3030(3)
_cell_length_b                   8.3030(3)
_cell_length_c                   20.3340(10)
_cell_measurement_reflns_used    4786
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      2.75
_cell_volume                     1214.01(9)
_computing_cell_refinement       'LSCELL (Clegg, 1997)'
_computing_data_collection       'Bruker AXS SMART'
_computing_data_reduction        'Bruker AXS SAINT'
_computing_molecular_graphics    X-STEP/DIAMOND
_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 glass fibre'
;
_diffrn_ambient_temperature      150(2)
_diffrn_crystal_treatment        'Flash cooled in nitrogen stream'
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device_type  'Bruker AXS SMART CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_radiation_source         'Daresbury SRS Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.68900
_diffrn_reflns_av_R_equivalents  0.0741
_diffrn_reflns_av_sigmaI/netI    0.0490
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            7609
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         2.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    4.051
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.425813
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 Mean and maximum errors in direction cosine check functions are 0.001
 and 0.006 respectively. 4786 reflections were employed for parameter 
 determination. R(int)= 0.0900 and R(int) = 0.0623 before and after the 
 refinements with final corrected 8458 reflections. The settings for 
 parameter refinements are (Intensity/sigma)threshold = 5.000 and 
 (Intensity + sigma)/(Mean intensity) threshold = 0.2500. And 2-theta
 dependent absorption correction was not applied.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    2.150
_exptl_crystal_description       platelet
_exptl_crystal_F_000             777
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.417
_refine_diff_density_min         -1.096
_refine_diff_density_rms         0.245
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     65
_refine_ls_number_reflns         1153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0867P)^2^+3.2068P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1388
_refine_ls_wR_factor_ref         0.1458
_reflns_number_gt                831
_reflns_number_total             1153
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0109848_1.cif
_cod_data_source_block           Co8(SO4)2(OH)12(dabco).2(H2O)
_cod_database_code               4115742