#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:39:21 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179487 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/84/4338431.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4338431
loop_
_publ_author_name
'Díaz-Gallifa, Pau'
'Fabelo, Oscar'
'Pasán, Jorge'
'Cañadillas-Delgado, Laura'
'Rodríguez-Carvajal, Juan'
'Lloret, Francesc'
'Julve, Miguel'
'Ruiz-Pérez, Catalina'
_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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0515P)²+1.1650P] where P=(Fo²+2Fc²)/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
#BEGIN Tags that were not found in dictionaries:
_exptl_absorpt_correction_t_ave  0.8618
#END Tags that were not found in dictionaries
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.44926(4) 0.17400(3) 0.51141(3) 0.00734(14) Uani 1 1 d .
Co2 Co 0.5000 0.5000 0.5000 0.00777(14) Uani 1 2 d S
Co3 Co 0.5000 0.5000 0.0000 0.01083(14) Uani 1 2 d S
C1 C 0.1805(3) 0.3348(2) -0.0045(2) 0.0092(4) Uani 1 1 d .
C2 C 0.1260(3) 0.3204(2) 0.1573(2) 0.0074(4) Uani 1 1 d .
H2 H 0.0421 0.4187 0.2092 0.009 Uiso 1 1 calc R
C3 C 0.0315(3) 0.1959(2) 0.2262(2) 0.0074(4) Uani 1 1 d .
H3 H 0.0606 0.1101 0.1548 0.009 Uiso 1 1 calc R
C4 C 0.2926(3) 0.2609(2) 0.2220(2) 0.0081(4) Uani 1 1 d .
H4 H 0.4099 0.1949 0.1476 0.010 Uiso 1 1 calc R
C5 C 0.1678(3) 0.1668(2) 0.3210(2) 0.0077(4) Uani 1 1 d .
H5 H 0.0961 0.2209 0.4191 0.009 Uiso 1 1 calc R
C6 C 0.2769(3) 0.0107(2) 0.3373(2) 0.0098(4) Uani 1 1 d .
C7 C 0.3481(3) 0.3786(2) 0.2894(2) 0.0085(4) Uani 1 1 d .
C8 C -0.1804(3) 0.2451(2) 0.3195(2) 0.0084(4) Uani 1 1 d .
O1 O 0.3844(3) 0.48459(19) 0.21746(17) 0.0188(4) Uani 1 1 d .
O2 O 0.3532(2) 0.36904(16) 0.41924(16) 0.0094(3) Uani 1 1 d .
O3 O 0.0809(3) 0.2957(2) -0.07020(18) 0.0219(4) Uani 1 1 d .
O4 O 0.3225(2) 0.38848(19) -0.06631(17) 0.0146(3) Uani 1 1 d .
O5 O 0.2413(3) -0.10041(19) 0.2969(2) 0.0256(4) Uani 1 1 d .
O6 O 0.4110(2) 0.00493(16) 0.39512(17) 0.0103(3) Uani 1 1 d .
O7 O -0.2477(2) 0.38173(18) 0.35996(19) 0.0170(3) Uani 1 1 d .
O8 O -0.2715(2) 0.14708(17) 0.35756(18) 0.0145(3) Uani 1 1 d .
O9W O 0.4926(2) 0.32601(16) 0.64691(16) 0.0105(3) Uani 1 1 d .
O10W O 0.1822(3) 0.1745(2) 0.66023(18) 0.0185(4) Uani 1 1 d .
O11W O 0.2917(3) 0.7121(2) 0.0276(2) 0.0215(4) Uani 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0040 0.0020 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0130 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3580 1.0350 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O10W Co1 O2 96.82(8) . .
O10W Co1 O6 85.78(7) . .
O2 Co1 O6 105.26(6) . .
O10W Co1 O6 90.82(7) . 2_656
O2 Co1 O6 169.02(6) . 2_656
O6 Co1 O6 83.10(6) . 2_656
O10W Co1 O8 173.52(6) . 1_655
O2 Co1 O8 88.48(7) . 1_655
O6 Co1 O8 89.24(7) . 1_655
O6 Co1 O8 84.47(7) 2_656 1_655
O10W Co1 O9W 91.93(7) . .
O2 Co1 O9W 81.35(6) . .
O6 Co1 O9W 173.21(6) . .
O6 Co1 O9W 90.54(6) 2_656 .
O8 Co1 O9W 92.55(7) 1_655 .
O7 Co2 O7 180.0 1_655 2_566
O7 Co2 O9W 91.99(7) 1_655 .
O7 Co2 O9W 88.01(7) 2_566 .
O7 Co2 O9W 88.01(7) 1_655 2_666
O7 Co2 O9W 91.99(7) 2_566 2_666
O9W Co2 O9W 180.0 . 2_666
O7 Co2 O2 88.89(7) 1_655 .
O7 Co2 O2 91.11(7) 2_566 .
O9W Co2 O2 78.79(6) . .
O9W Co2 O2 101.21(6) 2_666 .
O7 Co2 O2 91.11(7) 1_655 2_666
O7 Co2 O2 88.89(7) 2_566 2_666
O9W Co2 O2 101.21(6) . 2_666
O9W Co2 O2 78.79(6) 2_666 2_666
O2 Co2 O2 180.00(6) . 2_666
O1 Co3 O1 180.0 . 2_665
O1 Co3 O11W 87.61(8) . .
O1 Co3 O11W 92.39(8) 2_665 .
O1 Co3 O11W 92.39(8) . 2_665
O1 Co3 O11W 87.61(8) 2_665 2_665
O11W Co3 O11W 180.0 . 2_665
O1 Co3 O4 82.86(7) . 2_665
O1 Co3 O4 97.14(7) 2_665 2_665
O11W Co3 O4 87.30(7) . 2_665
O11W Co3 O4 92.70(7) 2_665 2_665
O1 Co3 O4 97.14(7) . .
O1 Co3 O4 82.86(7) 2_665 .
O11W Co3 O4 92.70(7) . .
O11W Co3 O4 87.30(7) 2_665 .
O4 Co3 O4 180.00(8) 2_665 .
O3 C1 O4 123.41(19) . .
O3 C1 C2 118.22(18) . .
O4 C1 C2 118.35(18) . .
C1 C2 C3 120.08(17) . .
C1 C2 C4 118.19(17) . .
C3 C2 C4 89.88(14) . .
C8 C3 C2 116.55(17) . .
C8 C3 C5 111.27(16) . .
C2 C3 C5 88.39(14) . .
C7 C4 C5 119.55(17) . .
C7 C4 C2 115.02(17) . .
C5 C4 C2 88.70(14) . .
C6 C5 C4 115.60(17) . .
C6 C5 C3 120.89(17) . .
C4 C5 C3 89.58(15) . .
O5 C6 O6 123.9(2) . .
O5 C6 C5 122.27(19) . .
O6 C6 C5 113.78(17) . .
O1 C7 O2 121.81(19) . .
O1 C7 C4 118.41(18) . .
O2 C7 C4 119.76(17) . .
O8 C8 O7 125.5(2) . .
O8 C8 C3 118.46(18) . .
O7 C8 C3 115.89(18) . .
C7 O1 Co3 131.78(15) . .
C7 O2 Co1 125.88(13) . .
C7 O2 Co2 120.63(13) . .
Co1 O2 Co2 96.55(6) . .
C1 O4 Co3 136.81(14) . .
C6 O6 Co1 128.77(14) . .
C6 O6 Co1 128.36(13) . 2_656
Co1 O6 Co1 96.90(6) . 2_656
C8 O7 Co2 132.63(15) . 1_455
C8 O8 Co1 127.56(14) . 1_455
Co1 O9W Co2 95.84(6) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O10W 2.0623(18) .
Co1 O2 2.0756(16) .
Co1 O6 2.0880(16) .
Co1 O6 2.0889(16) 2_656
Co1 O8 2.1039(18) 1_655
Co1 O9W 2.1073(16) .
Co2 O7 1.9908(19) 1_655
Co2 O7 1.9908(19) 2_566
Co2 O9W 2.1441(16) .
Co2 O9W 2.1441(16) 2_666
Co2 O2 2.1517(15) .
Co2 O2 2.1517(15) 2_666
Co3 O1 2.0326(17) .
Co3 O1 2.0326(17) 2_665
Co3 O11W 2.136(2) .
Co3 O11W 2.136(2) 2_665
Co3 O4 2.1424(16) 2_665
Co3 O4 2.1424(16) .
C1 O3 1.251(3) .
C1 O4 1.268(3) .
C1 C2 1.508(3) .
C2 C3 1.549(3) .
C2 C4 1.553(3) .
C3 C8 1.508(3) .
C3 C5 1.561(3) .
C4 C7 1.501(3) .
C4 C5 1.549(3) .
C5 C6 1.506(3) .
C6 O5 1.235(3) .
C6 O6 1.295(3) .
C7 O1 1.239(3) .
C7 O2 1.279(3) .
C8 O8 1.262(3) .
C8 O7 1.259(3) .
O6 Co1 2.0889(16) 2_656
O7 Co2 1.9908(19) 1_455
O8 Co1 2.1039(18) 1_455
