#------------------------------------------------------------------------------
#$Date: 2015-08-07 06:04:11 +0300 (Fri, 07 Aug 2015) $
#$Revision: 153034 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/09/2240977.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2240977
loop_
_publ_author_name
'Richers, Casseday P.'
'Bertke, Jeffery A.'
'Rauchfuss, Thomas B.'
_publ_contact_author
;
Jeffery A. Bertke
School of Chemical Sciences
University of Illinois at Urbana-Champaign
Urbana, Illinois  61801
USA
;
_publ_section_title
;
 Crystal structure of
 di-μ-hydroxido-κ⁴O:O-bis[bis(acetylacetonato-κ²O,O')cobalt(III)]
;
_journal_coeditor_code           WM5186
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              983
_journal_page_last               985
_journal_paper_doi               10.1107/S2056989015013663
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co2 (C5 H7 O2)4 (O H)2]'
_chemical_formula_moiety         'C20 H30 Co2 O10'
_chemical_formula_sum            'C20 H30 Co2 O10'
_chemical_formula_weight         548.30
_chemical_name_systematic
Di-μ-hydroxido-κ⁴O:O-bis[bis(acetylacetonato-κ²O,O')cobalt(III)]
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_cell_angle_alpha                100.786(8)
_cell_angle_beta                 106.708(8)
_cell_angle_gamma                99.492(9)
_cell_formula_units_Z            1
_cell_length_a                   7.8610(11)
_cell_length_b                   8.2481(11)
_cell_length_c                   9.8372(13)
_cell_measurement_reflns_used    3791
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.50
_cell_measurement_theta_min      2.58
_cell_volume                     583.67(14)
_computing_cell_refinement
;
SAINT (Bruker, 2013)
;
_computing_data_collection
;
APEX2 (Bruker, 2013)
;
_computing_data_reduction
;
SAINT (Bruker, 2013)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008), CrystalMaker (CrystalMaker, 1994)
;
_computing_publication_material
;
XCIF (Bruker, 2013) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL-2013/4 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device       'Bruker Kappa APEXII CCD'
_diffrn_measurement_method       'profile data from φ and ω 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  0.0834
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            16164
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.328
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    1.472
_exptl_absorpt_correction_T_max  0.94474
_exptl_absorpt_correction_T_min  0.77613
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2012)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             284
_exptl_crystal_size_max          0.227
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.042
_refine_diff_density_max         0.390
_refine_diff_density_min         -0.526
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     152
_refine_ls_number_reflns         2617
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0357
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0366P)²+0.1984P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0873
_refine_ls_wR_factor_ref         0.0929
_reflns_number_gt                2228
_reflns_number_total             2617
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            wm5186sup1.cif
_cod_data_source_block           I
_cod_database_code               2240977
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.731
_shelx_estimated_absorpt_t_max   0.941
_shelxl_version_number           2014/6
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
Co Co1 0.08356(4) 0.96491(4) 0.63894(3) 0.01839(12) Uani d 1
O O1 0.0955(2) 1.1492(2) 0.54669(18) 0.0197(4) Uani d 1
H H1 0.182(4) 1.158(4) 0.530(3) 0.030 Uiso d 1
O O2 0.0442(2) 0.7772(2) 0.71880(18) 0.0244(4) Uani d 1
O O3 0.2682(2) 0.9024(2) 0.56955(18) 0.0220(4) Uani d 1
C C1 0.0467(4) 0.5042(3) 0.7559(3) 0.0294(6) Uani d 1
H H1A 0.1238 0.5263 0.8584 0.044 Uiso calc 1
H H1B 0.0576 0.3969 0.7002 0.044 Uiso calc 1
H H1C -0.0808 0.4967 0.7508 0.044 Uiso calc 1
C C2 0.1074(3) 0.6460(3) 0.6920(2) 0.0216(5) Uani d 1
C C3 0.2293(3) 0.6301(3) 0.6154(3) 0.0239(5) Uani d 1
H H3 0.2605 0.5236 0.5962 0.029 Uiso calc 1
C C4 0.3092(3) 0.7594(3) 0.5647(2) 0.0204(5) Uani d 1
C C5 0.4588(3) 0.7360(3) 0.5010(3) 0.0291(6) Uani d 1
H H5A 0.4703 0.8171 0.4411 0.044 Uiso calc 1
H H5B 0.4290 0.6201 0.4398 0.044 Uiso calc 1
H H5C 0.5745 0.7556 0.5805 0.044 Uiso calc 1
O O4 -0.1041(2) 1.0298(2) 0.70365(18) 0.0211(3) Uani d 1
O O5 0.2764(2) 1.0871(2) 0.81009(18) 0.0258(4) Uani d 1
C C6 -0.2501(3) 1.1417(4) 0.8641(3) 0.0302(6) Uani d 1
H H6A -0.2682 1.2526 0.8490 0.045 Uiso calc 1
H H6B -0.2371 1.1397 0.9658 0.045 Uiso calc 1
H H6C -0.3556 1.0527 0.7980 0.045 Uiso calc 1
C C7 -0.0812(3) 1.1114(3) 0.8328(3) 0.0216(5) Uani d 1
C C8 0.0873(3) 1.1769(3) 0.9434(3) 0.0265(5) Uani d 1
H H8 0.0877 1.2323 1.0373 0.032 Uiso calc 1
C C9 0.2534(3) 1.1666(3) 0.9258(3) 0.0245(5) Uani d 1
C C10 0.4268(4) 1.2530(4) 1.0500(3) 0.0383(7) Uani d 1
H H10A 0.4992 1.1698 1.0733 0.057 Uiso calc 1
H H10B 0.3972 1.3033 1.1363 0.057 Uiso calc 1
H H10C 0.4973 1.3424 1.0215 0.057 Uiso calc 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 -1.00 2.00 0.0910
0.00 1.00 -2.00 0.0930
2.00 1.00 -1.00 0.0670
-2.00 -1.00 1.00 0.0690
0.00 -1.00 0.00 0.0200
0.00 1.00 0.00 0.0210
3.00 -1.00 0.00 0.0670
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O3 Co1 O4 . . 178.37(6)
O3 Co1 O5 . . 85.06(7)
O4 Co1 O5 . . 95.92(7)
O3 Co1 O2 . . 95.73(7)
O4 Co1 O2 . . 85.55(7)
O5 Co1 O2 . . 91.96(7)
O3 Co1 O1 . 2_576 90.26(7)
O4 Co1 O1 . 2_576 88.67(7)
O5 Co1 O1 . 2_576 173.53(7)
O2 Co1 O1 . 2_576 92.95(7)
O3 Co1 O1 . . 88.10(7)
O4 Co1 O1 . . 90.54(7)
O5 Co1 O1 . . 93.29(7)
O2 Co1 O1 . . 173.75(7)
O1 Co1 O1 2_576 . 82.07(7)
O3 Co1 Co1 . 2_576 88.91(5)
O4 Co1 Co1 . 2_576 89.47(5)
O5 Co1 Co1 . 2_576 134.10(5)
O2 Co1 Co1 . 2_576 133.93(6)
O1 Co1 Co1 2_576 2_576 41.09(5)
O1 Co1 Co1 . 2_576 40.98(5)
Co1 O1 Co1 2_576 . 97.93(7)
Co1 O1 H1 2_576 . 103(2)
Co1 O1 H1 . . 106(2)
C2 O2 Co1 . . 123.65(15)
C4 O3 Co1 . . 124.41(15)
C2 C1 H1A . . 109.5
C2 C1 H1B . . 109.5
H1A C1 H1B . . 109.5
C2 C1 H1C . . 109.5
H1A C1 H1C . . 109.5
H1B C1 H1C . . 109.5
O2 C2 C3 . . 125.1(2)
O2 C2 C1 . . 115.2(2)
C3 C2 C1 . . 119.6(2)
C2 C3 C4 . . 124.5(2)
C2 C3 H3 . . 117.8
C4 C3 H3 . . 117.8
O3 C4 C3 . . 125.0(2)
O3 C4 C5 . . 115.1(2)
C3 C4 C5 . . 120.0(2)
C4 C5 H5A . . 109.5
C4 C5 H5B . . 109.5
H5A C5 H5B . . 109.5
C4 C5 H5C . . 109.5
H5A C5 H5C . . 109.5
H5B C5 H5C . . 109.5
C7 O4 Co1 . . 124.45(16)
C9 O5 Co1 . . 123.82(16)
C7 C6 H6A . . 109.5
C7 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
C7 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 109.5
O4 C7 C8 . . 125.1(2)
O4 C7 C6 . . 116.0(2)
C8 C7 C6 . . 118.9(2)
C9 C8 C7 . . 124.4(2)
C9 C8 H8 . . 117.8
C7 C8 H8 . . 117.8
O5 C9 C8 . . 125.7(2)
O5 C9 C10 . . 114.7(2)
C8 C9 C10 . . 119.6(2)
C9 C10 H10A . . 109.5
C9 C10 H10B . . 109.5
H10A C10 H10B . . 109.5
C9 C10 H10C . . 109.5
H10A C10 H10C . . 109.5
H10B C10 H10C . . 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O3 . 1.8770(16)
Co1 O4 . 1.8814(16)
Co1 O5 . 1.8820(17)
Co1 O2 . 1.8830(16)
Co1 O1 2_576 1.9087(17)
Co1 O1 . 1.9131(16)
Co1 Co1 2_576 2.8829(7)
O1 Co1 2_576 1.9087(17)
O1 H1 . 0.74(3)
O2 C2 . 1.278(3)
O3 C4 . 1.269(3)
C1 C2 . 1.502(3)
C1 H1A . 0.9800
C1 H1B . 0.9800
C1 H1C . 0.9800
C2 C3 . 1.387(3)
C3 C4 . 1.393(3)
C3 H3 . 0.9500
C4 C5 . 1.506(3)
C5 H5A . 0.9800
C5 H5B . 0.9800
C5 H5C . 0.9800
O4 C7 . 1.268(3)
O5 C9 . 1.279(3)
C6 C7 . 1.495(3)
C6 H6A . 0.9800
C6 H6B . 0.9800
C6 H6C . 0.9800
C7 C8 . 1.395(3)
C8 C9 . 1.380(3)
C8 H8 . 0.9500
C9 C10 . 1.502(3)
C10 H10A . 0.9800
C10 H10B . 0.9800
C10 H10C . 0.9800
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
C1 H1B O1 1_545 0.98 2.42 3.395(3) 174.0

_cod_database_fobs_code 2240977
