Synthesis, Crystal Structure, and Magnetic Characterization of the Three-Dimensional Compound [Co2(cbut)(H2O)3]n (H4cbut = 1,2,3,4-Cyclobutanetetracarboxylic Acid).
Díaz-Gallifa, Pau; Fabelo, Oscar; Pasán, Jorge; Cañadillas-Delgado, Laura; Rodríguez-Carvajal, Juan; Lloret, Francesc; Julve, Miguel; Ruiz-Pérez, Catalina; Inorganic chemistry 53 (2014) 5674–5683; doi:10.1021/ic500443t

data_4338431
_publ_section_title
;
 Synthesis, Crystal Structure, and Magnetic Characterization of the
 Three-Dimensional Compound [Co2(cbut)(H2O)3]n (H4cbut =
 1,2,3,4-Cyclobutanetetracarboxylic Acid).
;
_journal_issue                   11
_journal_name_full               'Inorganic chemistry'
_journal_page_first              5674
_journal_page_last               5683
_journal_paper_doi               10.1021/ic500443t
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C8 H10 Co2 O11'
_chemical_formula_weight         400.02
_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                89.01(3)
_cell_angle_beta                 71.16(3)
_cell_angle_gamma                74.82(3)
_cell_formula_units_Z            2
_cell_length_a                   7.5240(15)
_cell_length_b                   9.3200(19)
_cell_length_c                   9.7440(19)
_cell_measurement_temperature    100(2)
_cell_volume                     622.4(3)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'MxCube (ESRF, 2006)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 9.6
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Single-axis HUBER diffractometer'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_detector       'ADSC Q210r CCD (binned mode)'
_diffrn_radiation_monochromator  'Si 111'
_diffrn_radiation_wavelength     0.73830
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10085
_diffrn_reflns_theta_full        27.73
_diffrn_reflns_theta_max         27.73
_diffrn_reflns_theta_min         3.34
_diffrn_source                   synchrotron
_diffrn_source_type              'ESRF-CRG BM16'
_exptl_absorpt_coefficient_mu    2.980
_exptl_absorpt_correction_T_max  0.8620
_exptl_absorpt_correction_T_min  0.8614
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             400
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_size_rad          0.0500
_refine_diff_density_max         0.790
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       0.047(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     194
_refine_ls_number_reflns         2572
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.926
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0515P)^2^+1.1650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0854
_refine_ls_wR_factor_ref         0.0871
_reflns_number_gt                2533
_reflns_number_total             2572
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500443t_si_002.cif
_cod_data_source_block           cbut_Co(II)
_cod_depositor_comments          'Adding full bibliography for 4338431.cif.'
_cod_original_cell_volume        622.4(2)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4338431
_exptl_absorpt_correction_t_ave  0.8618