#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/85/2238531.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_2238531
loop_
_publ_author_name
'Benslimane, Meriem'
'Redjel, Yasmine Kheira'
'Dénès, Georges'
'Merazig, Hocine'
_publ_section_title
;
 Tetrakis(μ-2-phenylacetato-κ²O:O')bis{[4-(dimethylamino)pyridine-κN¹]cobalt(II)}
;
_journal_coeditor_code           LR2113
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m517
_journal_page_last               m518
_journal_paper_doi               10.1107/S1600536813023258
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Co2 (C8 H7 O2)4 (C7 H10 N2)2]'
_chemical_formula_moiety         'C46 H48 Co2 N4 O8'
_chemical_formula_sum            'C46 H48 Co2 N4 O8'
_chemical_formula_weight         902.74
_chemical_name_systematic
Tetrakis(μ-2-phenylacetato-κ²O:O')bis{[4-(dimethylamino)pyridine-κN¹]cobalt(II)}
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                99.766(5)
_cell_angle_beta                 101.878(5)
_cell_angle_gamma                105.335(5)
_cell_formula_units_Z            1
_cell_length_a                   8.107(5)
_cell_length_b                   11.043(5)
_cell_length_c                   12.573(5)
_cell_measurement_reflns_used    4872
_cell_measurement_temperature    150
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.28
_cell_volume                     1031.9(9)
_computing_cell_refinement       'SAINT (Bruker, 2012)'
_computing_data_collection       'APEX2 (Bruker, 2012)'
_computing_data_reduction        'SAINT (Bruker, 2012)'
_computing_molecular_graphics
'ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω and φ'
_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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9238
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    0.864
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2012)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.453
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       box
_exptl_crystal_F_000             470
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.252
_refine_diff_density_min         -0.244
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         3645
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0281
_refine_ls_R_factor_gt           0.025
_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/[σ²(Fo²)+(0.0206P)²+0.6871P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0601
_reflns_number_gt                3352
_reflns_number_total             3645
_reflns_threshold_expression     I>2σ(I))
_cod_data_source_file            lr2113.cif
_cod_data_source_block           I
_cod_database_code               2238531
_cod_database_fobs_code          2238531
loop_
_symmetry_equiv_pos_as_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_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Co Co1 0.56888(3) 0.01135(2) 0.114253(18) 0.01603(8) Uani d . 1 1
O O1 0.70384(17) 0.18802(11) 0.09742(10) 0.0256(3) Uani d . 1 1
O O3 0.75242(16) -0.06983(12) 0.07678(10) 0.0241(3) Uani d . 1 1
O O2 0.59969(17) 0.17191(12) -0.08452(10) 0.0248(3) Uani d . 1 1
O O4 0.64516(17) -0.08060(13) -0.10383(10) 0.0277(3) Uani d . 1 1
N N1 0.7414(2) 0.15583(15) 0.63408(12) 0.0259(3) Uani d . 1 1
N N2 0.64381(19) 0.06270(13) 0.28539(11) 0.0178(3) Uani d . 1 1
C C10 0.7997(2) 0.46694(16) 0.12315(14) 0.0192(4) Uani d . 1 1
C C3 0.7158(2) -0.00546(16) 0.34964(14) 0.0197(4) Uani d . 1 1
H H3 0.7415 -0.0764 0.3139 0.024 Uiso calc R 1 1
C C11 0.7164(3) 0.55861(17) 0.10444(16) 0.0256(4) Uani d . 1 1
H H11 0.6661 0.5599 0.0313 0.031 Uiso calc R 1 1
C C1 0.7158(2) 0.12779(17) 0.52207(14) 0.0195(4) Uani d . 1 1
C C18 0.8183(2) -0.25048(16) -0.17600(14) 0.0181(4) Uani d . 1 1
C C13 0.7818(3) 0.64805(18) 0.30092(16) 0.0302(4) Uani d . 1 1
H H13 0.7766 0.7085 0.3603 0.036 Uiso calc R 1 1
C C17 0.8651(2) -0.18185(17) -0.05447(14) 0.0205(4) Uani d . 1 1
H H17A 0.9855 -0.1236 -0.0338 0.025 Uiso calc R 1 1
H H17B 0.8624 -0.2454 -0.0097 0.025 Uiso calc R 1 1
C C23 0.9124(2) -0.20046(17) -0.24739(15) 0.0222(4) Uani d . 1 1
H H23 1.0052 -0.1233 -0.2202 0.027 Uiso calc R 1 1
C C2 0.7540(2) 0.02208(17) 0.46401(14) 0.0216(4) Uani d . 1 1
H H2 0.8051 -0.0289 0.5033 0.026 Uiso calc R 1 1
C C19 0.6790(2) -0.36483(17) -0.21909(15) 0.0245(4) Uani d . 1 1
H H19 0.6135 -0.399 -0.1724 0.029 Uiso calc R 1 1
C C9 0.8102(3) 0.37074(16) 0.02588(15) 0.0236(4) Uani d . 1 1
H H9A 0.9324 0.3717 0.0358 0.028 Uiso calc R 1 1
H H9B 0.7754 0.3982 -0.0424 0.028 Uiso calc R 1 1
C C14 0.8655(3) 0.55707(19) 0.32101(16) 0.0311(4) Uani d . 1 1
H H14 0.9163 0.5563 0.3942 0.037 Uiso calc R 1 1
C C4 0.6139(2) 0.16674(17) 0.34079(14) 0.0228(4) Uani d . 1 1
H H4 0.568 0.2179 0.299 0.027 Uiso calc R 1 1
C C15 0.8741(2) 0.46726(18) 0.23306(15) 0.0267(4) Uani d . 1 1
H H15 0.9303 0.4063 0.2476 0.032 Uiso calc R 1 1
C C5 0.6466(2) 0.20198(17) 0.45452(15) 0.0246(4) Uani d . 1 1
H H5 0.6231 0.2753 0.4876 0.029 Uiso calc R 1 1
C C22 0.8696(3) -0.26441(19) -0.35918(15) 0.0274(4) Uani d . 1 1
H H22 0.934 -0.23 -0.4062 0.033 Uiso calc R 1 1
C C16 0.7435(2) -0.10501(16) -0.02568(14) 0.0180(4) Uani d . 1 1
C C20 0.6361(3) -0.42857(18) -0.33028(16) 0.0291(4) Uani d . 1 1
H H20 0.5425 -0.5053 -0.3579 0.035 Uiso calc R 1 1
C C12 0.7061(3) 0.64871(18) 0.19226(17) 0.0322(5) Uani d . 1 1
H H12 0.6487 0.7091 0.178 0.039 Uiso calc R 1 1
C C8 0.6943(2) 0.23260(16) 0.01192(14) 0.0186(4) Uani d . 1 1
C C7 0.8177(3) 0.0810(2) 0.70317(16) 0.0328(5) Uani d . 1 1
H H7A 0.8256 0.1152 0.7802 0.049 Uiso calc R 1 1
H H7B 0.9341 0.0858 0.6946 0.049 Uiso calc R 1 1
H H7C 0.7438 -0.0076 0.6804 0.049 Uiso calc R 1 1
C C21 0.7319(3) -0.37875(19) -0.40079(15) 0.0292(4) Uani d . 1 1
H H21 0.7037 -0.4219 -0.4756 0.035 Uiso calc R 1 1
C C6 0.6940(3) 0.2633(2) 0.68950(16) 0.0353(5) Uani d . 1 1
H H6A 0.721 0.2693 0.7686 0.053 Uiso calc R 1 1
H H6B 0.5694 0.2493 0.6611 0.053 Uiso calc R 1 1
H H6C 0.7601 0.3421 0.6754 0.053 Uiso calc R 1 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'
N N 0.0061 0.0033 '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_
_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 O1 . . 93.27(6)
O3 Co1 O2 . 2_655 87.33(6)
O1 Co1 O2 . 2_655 163.77(5)
O3 Co1 N2 . . 102.92(6)
O1 Co1 N2 . . 94.29(5)
O2 Co1 N2 2_655 . 101.39(5)
O3 Co1 O4 . 2_655 163.73(5)
O1 Co1 O4 . 2_655 85.64(6)
O2 Co1 O4 2_655 2_655 89.27(7)
N2 Co1 O4 . 2_655 93.35(5)
O3 Co1 Co1 . 2_655 89.34(4)
O1 Co1 Co1 . 2_655 79.04(4)
O2 Co1 Co1 2_655 2_655 84.75(4)
N2 Co1 Co1 . 2_655 166.44(4)
O4 Co1 Co1 2_655 2_655 74.50(4)
C8 O1 Co1 . . 129.17(11)
C16 O3 Co1 . . 116.62(11)
C8 O2 Co1 . 2_655 121.65(11)
C16 O4 Co1 . 2_655 133.30(12)
C1 N1 C6 . . 120.56(16)
C1 N1 C7 . . 121.55(16)
C6 N1 C7 . . 117.89(15)
C3 N2 C4 . . 115.61(15)
C3 N2 Co1 . . 124.00(11)
C4 N2 Co1 . . 120.31(11)
C11 C10 C15 . . 118.12(17)
C11 C10 C9 . . 120.35(16)
C15 C10 C9 . . 121.52(16)
N2 C3 C2 . . 124.67(16)
N2 C3 H3 . . 117.7
C2 C3 H3 . . 117.7
C10 C11 C12 . . 121.52(18)
C10 C11 H11 . . 119.2
C12 C11 H11 . . 119.2
N1 C1 C2 . . 122.71(16)
N1 C1 C5 . . 122.05(16)
C2 C1 C5 . . 115.23(16)
C23 C18 C19 . . 118.53(16)
C23 C18 C17 . . 120.81(16)
C19 C18 C17 . . 120.66(16)
C12 C13 C14 . . 119.66(18)
C12 C13 H13 . . 120.2
C14 C13 H13 . . 120.2
C18 C17 C16 . . 114.52(14)
C18 C17 H17A . . 108.6
C16 C17 H17A . . 108.6
C18 C17 H17B . . 108.6
C16 C17 H17B . . 108.6
H17A C17 H17B . . 107.6
C18 C23 C22 . . 120.65(17)
C18 C23 H23 . . 119.7
C22 C23 H23 . . 119.7
C3 C2 C1 . . 119.85(16)
C3 C2 H2 . . 120.1
C1 C2 H2 . . 120.1
C20 C19 C18 . . 120.91(17)
C20 C19 H19 . . 119.5
C18 C19 H19 . . 119.5
C10 C9 C8 . . 114.21(14)
C10 C9 H9A . . 108.7
C8 C9 H9A . . 108.7
C10 C9 H9B . . 108.7
C8 C9 H9B . . 108.7
H9A C9 H9B . . 107.6
C15 C14 C13 . . 120.40(18)
C15 C14 H14 . . 119.8
C13 C14 H14 . . 119.8
N2 C4 C5 . . 124.16(16)
N2 C4 H4 . . 117.9
C5 C4 H4 . . 117.9
C14 C15 C10 . . 120.78(17)
C14 C15 H15 . . 119.6
C10 C15 H15 . . 119.6
C4 C5 C1 . . 120.39(16)
C4 C5 H5 . . 119.8
C1 C5 H5 . . 119.8
C21 C22 C23 . . 120.28(18)
C21 C22 H22 . . 119.9
C23 C22 H22 . . 119.9
O4 C16 O3 . . 125.35(16)
O4 C16 C17 . . 118.12(15)
O3 C16 C17 . . 116.52(15)
C19 C20 C21 . . 120.23(18)
C19 C20 H20 . . 119.9
C21 C20 H20 . . 119.9
C13 C12 C11 . . 119.52(18)
C13 C12 H12 . . 120.2
C11 C12 H12 . . 120.2
O1 C8 O2 . . 125.30(16)
O1 C8 C9 . . 117.19(15)
O2 C8 C9 . . 117.50(15)
N1 C7 H7A . . 109.5
N1 C7 H7B . . 109.5
H7A C7 H7B . . 109.5
N1 C7 H7C . . 109.5
H7A C7 H7C . . 109.5
H7B C7 H7C . . 109.5
C22 C21 C20 . . 119.40(17)
C22 C21 H21 . . 120.3
C20 C21 H21 . . 120.3
N1 C6 H6A . . 109.5
N1 C6 H6B . . 109.5
H6A C6 H6B . . 109.5
N1 C6 H6C . . 109.5
H6A C6 H6C . . 109.5
H6B C6 H6C . . 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 . 2.0224(15)
Co1 O1 . 2.0382(14)
Co1 O2 2_655 2.0429(15)
Co1 N2 . 2.0460(16)
Co1 O4 2_655 2.0628(16)
Co1 Co1 2_655 2.8020(12)
O1 C8 . 1.253(2)
O3 C16 . 1.262(2)
O2 C8 . 1.256(2)
O2 Co1 2_655 2.0429(15)
O4 C16 . 1.247(2)
O4 Co1 2_655 2.0628(16)
N1 C1 . 1.349(2)
N1 C6 . 1.453(2)
N1 C7 . 1.454(2)
N2 C3 . 1.343(2)
N2 C4 . 1.345(2)
C10 C11 . 1.383(3)
C10 C15 . 1.388(3)
C10 C9 . 1.510(2)
C3 C2 . 1.369(2)
C3 H3 . 0.93
C11 C12 . 1.387(3)
C11 H11 . 0.93
C1 C2 . 1.410(2)
C1 C5 . 1.411(2)
C18 C23 . 1.386(2)
C18 C19 . 1.388(3)
C18 C17 . 1.506(2)
C13 C12 . 1.380(3)
C13 C14 . 1.382(3)
C13 H13 . 0.93
C17 C16 . 1.519(2)
C17 H17A . 0.97
C17 H17B . 0.97
C23 C22 . 1.388(3)
C23 H23 . 0.93
C2 H2 . 0.93
C19 C20 . 1.381(3)
C19 H19 . 0.93
C9 C8 . 1.524(2)
C9 H9A . 0.97
C9 H9B . 0.97
C14 C15 . 1.381(3)
C14 H14 . 0.93
C4 C5 . 1.366(2)
C4 H4 . 0.93
C15 H15 . 0.93
C5 H5 . 0.93
C22 C21 . 1.380(3)
C22 H22 . 0.93
C20 C21 . 1.384(3)
C20 H20 . 0.93
C12 H12 . 0.93
C7 H7A . 0.96
C7 H7B . 0.96
C7 H7C . 0.96
C21 H21 . 0.93
C6 H6A . 0.96
C6 H6B . 0.96
C6 H6C . 0.96
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
_geom_hbond_publ_flag
C6 H6A O2 1_556 0.9600 2.5300 3.337(3) 142.00 yes
C23 H23 O3 2_755 0.9300 2.5800 3.469(3) 159.00 yes
